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The accuracy of blood glucose measurement in clinical laboratories is vital for diabetes diagnosis. Trueness Verification Plan was carried out and analyzed for evaluating the standardization of serum glucose among clinical laboratories.

Even though reliable glucose concentration measurements are essential in diagnosis and monitoring of diabetes mellitus, external quality assurance based on mandatory reference method values can only be conducted to a limited extent for measurements in whole blood. The reason is the lack of stabilized whole blood materials suitable for the application in glucose measurement devices used in near-patient testing.

Street food outlets are characterised by poor microbiological quality of the food and poor hygiene practices that pose a risk to consumer health. The aim of the study was to evaluate the hygiene of surfaces in food trucks (FT) using the reference method together with alternatives such as PetrifilmTM and the bioluminescence method. TVC, S. aureus, Enterobacteriaceae, E. coli, L. monocytogenes, and Salmonella spp. were assessed. The material for the study consisted of swabs and prints taken from five surfaces (refrigeration, knife, cutting board, serving board, and working board) in 20 food trucks in Poland. In 13 food trucks, the visual assessment of hygiene was very good or good, but in 6 FTs, TVC was found to exceed log 3 CFU/100 cm2 on various surfaces. The assessment of surface hygiene using various methods in the food trucks did not demonstrate the substitutability of culture methods. PetrifilmTM tests were shown to be a convenient and reliable tool for the monitoring of mobile catering hygiene. No correlation was found between the subjective visual method and the measurement of adenosine 5-triphosphate. In order to reduce the risk of food infections caused by bacteria in food trucks, it is important to introduce detailed requirements for the hygiene practices used in food trucks, including techniques for monitoring the cleanliness of surfaces coming into contact with food, in particular cutting boards and work surfaces. Efforts should be focused on introducing mandatory, certified training for food truck personnel in the field of microbiological hazards, appropriate methods of hygienisation, and hygiene monitoring. [ABSTRACT FROM AUTHOR]

Abstract Blood glucose measurement is one of the most commonly performed clinical diagnostic tests used to monitor glycaemia in several animal diseases. Usually, these laboratory analyses are performed on blood venous samples in remote laboratories, and the results are delayed, at best. The use of portable glucometers could evidently solve many constraints but veterinary‐use glucometers are not usually available. The present study aimed to compare blood glucose levels obtained by Bionime glucometer to the reference method using glucose oxidase. Venous blood was collected from a total number of 140 healthy dogs (72 males and 68 females), of different breeds (28 German Shepherd, 27 Pitt bull, 21 Boxer, 24 Rottweiler and 40 cross‐bred dogs) and different ages (range: 3 months–14 years) for glucose measurement using the reference laboratory method. Capillary blood samples were used to conduct a glucose measurement with a human‐use glucometer. Our results revealed that there was no significant difference between the mean capillary blood glucose (CBG) measured with the human‐use glucometer (5.06 ± 0.84 mmol/L) and the mean venous blood glucose (VBG) measured with the laboratory reference method (4.90 ± 0.73 mmol/L) (p = 0.42). Similarly, there was no significant difference of the mean CBG and VBG in male dogs (5.11 ± 0.88 and 4.97 ± 0.75 mmol/L, respectively) and female dogs (5.01 ± 0.81 and 5.07 ± 0.72 mmol/L, respectively) (p = 0.73 and 0.21, respectively), and no correlation to neither age (5.43 ± 0.90 and 5.20 ± 0.70 mmol/L in 3 to 6 month‐old dogs, 5.03 ± 0.82 and 4.94 ± 0.79 mmol/L in 6 months to 1 year‐old, 4.94 ± 0.67 and 5.13 ± 0.66 mmol/L in 1 to 4 year‐old dogs; 4.88 ± 0.94 and 4.80 ± 0.75 mmol/L in dogs older than 4 years, respectively, p

The aims of this study were to determine the concentrations and elemental composition of PM10 in the village of Kotórz Mały (Poland), to analyse their seasonal variability, to determine the sources of pollutant emissions and to compare the consistency of the results obtained using different methods. Sampling and weather condition measurements were carried out in the winter (January–February) and spring (April) of 2019. Two combinations of different techniques were used to examine PM10 concentrations and their chemical composition: gravimetric method + atomic absorption spectrometry (GM+AAS) and continuous particle monitor + energy dispersive X-ray fluorescence (CPM+EDXRF). In winter, the average concentrations of PM10 measured by the GM and CPM were similar (GM 44.3 µg/m3; CPM 34.0 µg/m3), while in spring they were clearly different (GM 49.5 µg/m3; CPM 29.8 µg/m3). Both AAS and EDXRF proved that in both seasons, Ca, K and Fe had the highest shares in the PM10 mass. In the case of the lowest shares, the indications of the two methods were slightly different. Factor analysis indicated that air quality in the receptor was determined by soil erosion, coal and burning biomass, and the combustion of fuels in car engines; in the spring, air quality was also affected by gardening activities. [ABSTRACT FROM AUTHOR]

Railway superstructure components are subject to impact forces caused by irregularities in the rail and wheel or variations in the support stiffness. These imperfections lead to the premature and accelerated deterioration of the track and increase maintenance costs. Generally, to mitigate these dynamic loads, elastomeric rail pads are interposed between rails and sleepers. For each track section, the pad choice is made according to its stiffness, impact attenuation and cost. In this experimental study, eight types of rail pads were characterized using two procedures from EN 13146–3. The results revealed that the rail pad material and geometry affect the impact attenuation ability of the pad and the testing procedure affect the results. It was found that the preload applied is one of the parameters that most affects the impact attenuation value. Appling a preload of 50 kN during the impact attenuation test, which is suggested by the standard, affected this parameter by ranging from between ~2 and ~ 20, depending on the rail pad. Based on these results it is considered that EN 13146–3 should be updated. [ABSTRACT FROM AUTHOR]

A collaborative interlaboratory study of the method of direct determination of volatile compounds in spirit drinks and alcoholic products was performed. The proposed method employs ethanol, the major volatile component of an alcoholic product, as an internal standard. For the experiment realization, 9 laboratories from 4 countries – Belarus, Czech Republic, Turkey, Russia – were supplied with standard solutions for gas chromatographic measurements. Five aqueous ethanol 40 % (v/v) standard solutions containing target compounds in concentrations ranging from 10 to 400 mg/L of absolute alcohol were gravimetrically prepared and delivered to the participants. The interlaboratory study was evaluated according to the ISO 5725 standards and the «EuroChem» guide. The repeatability limits (within-laboratory precision) varied between 0.4 and 7.5 % for all samples and compounds, showing a sufficiently high repeatability of the method. The reproducibility limits (between-laboratory precision) were found to vary within a satisfactory range of 0.5–10.0 %. Precision of the method was well within the range predicted by the Horwitz equation for all analytes. In the study experimental estimation of trueness was performed for the first time. Analysis of the obtained results showed that the bias of the method is insignificant at the significance level 5 %. The experimentally determined concentrations of the analytes compared well to the gravimetrical values, thus showing very satisfactory accuracy of the method. The results of the interlaboratory study confirmed that the method «ethanol as internal standard» is robust and reliable and can be used as a standard method for the determination of volatile compounds in water-ethanol samples. Moreover, this method can be validated in any one laboratory without performing additional experimental studies based on the results obtained by validation of the traditional method.

Street food outlets are characterised by poor microbiological quality of the food and poor hygiene practices that pose a risk to consumer health. The aim of the study was to evaluate the hygiene of surfaces in food trucks (FT) using the reference method together with alternatives such as PetrifilmTM and the bioluminescence method. TVC, S. aureus, Enterobacteriaceae, E. coli, L. monocytogenes, and Salmonella spp. were assessed. The material for the study consisted of swabs and prints taken from five surfaces (refrigeration, knife, cutting board, serving board, and working board) in 20 food trucks in Poland. In 13 food trucks, the visual assessment of hygiene was very good or good, but in 6 FTs, TVC was found to exceed log 3 CFU/100 cm2 on various surfaces. The assessment of surface hygiene using various methods in the food trucks did not demonstrate the substitutability of culture methods. PetrifilmTM tests were shown to be a convenient and reliable tool for the monitoring of mobile catering hygiene. No correlation was found between the subjective visual method and the measurement of adenosine 5-triphosphate. In order to reduce the risk of food infections caused by bacteria in food trucks, it is important to introduce detailed requirements for the hygiene practices used in food trucks, including techniques for monitoring the cleanliness of surfaces coming into contact with food, in particular cutting boards and work surfaces. Efforts should be focused on introducing mandatory, certified training for food truck personnel in the field of microbiological hazards, appropriate methods of hygienisation, and hygiene monitoring.

Blood glucose measurement is one of the most commonly performed clinical diagnostic tests used to monitor glycaemia in several animal diseases. Usually, these laboratory analyses are performed on blood venous samples in remote laboratories, and the results are delayed, at best. The use of portable glucometers could evidently solve many constraints but veterinary‐use glucometers are not usually available. The present study aimed to compare blood glucose levels obtained by Bionime glucometer to the reference method using glucose oxidase. Venous blood was collected from a total number of 140 healthy dogs (72 males and 68 females), of different breeds (28 German Shepherd, 27 Pitt bull, 21 Boxer, 24 Rottweiler and 40 cross‐bred dogs) and different ages (range: 3 months–14 years) for glucose measurement using the reference laboratory method. Capillary blood samples were used to conduct a glucose measurement with a human‐use glucometer. Our results revealed that there was no significant difference between the mean capillary blood glucose (CBG) measured with the human‐use glucometer (5.06 ± 0.84 mmol/L) and the mean venous blood glucose (VBG) measured with the laboratory reference method (4.90 ± 0.73 mmol/L) (p = 0.42). Similarly, there was no significant difference of the mean CBG and VBG in male dogs (5.11 ± 0.88 and 4.97 ± 0.75 mmol/L, respectively) and female dogs (5.01 ± 0.81 and 5.07 ± 0.72 mmol/L, respectively) (p = 0.73 and 0.21, respectively), and no correlation to neither age (5.43 ± 0.90 and 5.20 ± 0.70 mmol/L in 3 to 6 month‐old dogs, 5.03 ± 0.82 and 4.94 ± 0.79 mmol/L in 6 months to 1 year‐old, 4.94 ± 0.67 and 5.13 ± 0.66 mmol/L in 1 to 4 year‐old dogs; 4.88 ± 0.94 and 4.80 ± 0.75 mmol/L in dogs older than 4 years, respectively, p < 0.05), nor to breed (4.94 ± 1.01 and 4.99 ± 0.79 mmol/L in German Shepherd, 5.13 ± 0.84 and 4.99 ± 0.79 mmol/L in Pitt Bull, 5.07 ± 0.94 and 5.07 ± 0.77 mmol/L in Boxer, 5.40 ± 0.59 and 5.48 ± 0.55 mmol/L in Rottweiler and 4.89 ± 0.75 and 4.77 ± 0.59 mmol/L in cross‐bred dogs, respectively, p < 0.05). The present study confirms that human glucometer can be used to measure glucose in dogs with a good accuracy. [ABSTRACT FROM AUTHOR]

Objectives: In 2009, the Japan Society of Clinical Chemistry (JSCC) recommended a reference method for the measurement of serum high-density lipoprotein cholesterol (HDL-C) and low-density lipoprotein cholesterol (LDL-C) levels. This automated method uses cholesterol esterase-cholesterol dehydrogenase to measure cholesterol levels in fractions obtained after ultracentrifugation and dextran sulfate/magnesium chloride precipitation. In the present study, using fresh samples, we compared the LDL-C and HDL-C levels measured using this method with those measured using the traditional Centers for Disease Control and Prevention (CDC)-beta-quantification (BQ) method. Design: and methods: Using both the JSCC and CDC-BQ methods, LDL-C/HDL-C levels were measured in 47 non-diseased and 126 diseased subjects, whose triglyceride levels were lower than 11.29 ​mmol/L (1000 ​mg/dL). Results: For LDL-C, the equation of the line representing the correlation between the two methods was y ​= ​0.991x + 0.009 ​mmol/L; r ​= ​0.999; and Sy/x ​= ​0.025 ​mmol/L, where x is the mean LDL-C level measured using the CDC-BQ method. Similarly, for HDL-C, the equation of the line representing the correlation between the two methods was y ​= ​0.988x + 0.041 ​mmol/L, r ​= ​0.999, and Sy/x ​= ​0.019 ​mmol/L, where x is the mean HDL-C level measured using the CDC-BQ method. Conclusions: The JSCC method agreed with the CDC-BQ method in cases of both non-diseased and diseased subjects, including those with dyslipidemia.

The aims of this study were to determine the concentrations and elemental composition of PM10 in the village of Kotórz Mały (Poland), to analyse their seasonal variability, to determine the sources of pollutant emissions and to compare the consistency of the results obtained using different methods. Sampling and weather condition measurements were carried out in the winter (January–February) and spring (April) of 2019. Two combinations of different techniques were used to examine PM10 concentrations and their chemical composition: gravimetric method + atomic absorption spectrometry (GM+AAS) and continuous particle monitor + energy dispersive X-ray fluorescence (CPM+EDXRF). In winter, the average concentrations of PM10 measured by the GM and CPM were similar (GM 44.3 µg/m3; CPM 34.0 µg/m3), while in spring they were clearly different (GM 49.5 µg/m3; CPM 29.8 µg/m3). Both AAS and EDXRF proved that in both seasons, Ca, K and Fe had the highest shares in the PM10 mass. In the case of the lowest shares, the indications of the two methods were slightly different. Factor analysis indicated that air quality in the receptor was determined by soil erosion, coal and burning biomass, and the combustion of fuels in car engines; in the spring, air quality was also affected by gardening activities.

Nitric oxide (NO) and its by-products are important biological signals in human physiology and pathology particularly in the vascular and immune systems. Thus, in situ determination of the NO-related molecule (NOx) levels using embedded sensors is of high importance particularly in the context of cellular biocompatibility testing. However, NOx analytical reference method dedicated to the evaluation of biomaterial biocompatibility testing is lacking. Herein, we demonstrate a PAPA-NONOate-based reference method for the calibration of NOx sensors. After, the validation of this reference method and its potentialities were demonstrated for the detection of the oxidative stress-related NO secretion of vascular endothelial cells in a 3D tissue issued from 3D printing. Such NOx detection method can be an integral part of cell response to biomaterials. [ABSTRACT FROM AUTHOR]

Several methods are used worldwide for antibiotic susceptibility testing (AST) for the Mycobacterium tuberculosis complex (MTBC). The variability in the results obtained with these methods hampers setting epidemiological cut-off (ECOFF) values and clinical breakpoints according to EUCAST guidelines. Methods for susceptibility testing and determination of the minimal inhibitory concentrations (MICs) need to be standardized for MTBC isolates for old and new agents. Our objective was to establish a standardized reference method for MIC determination for MTBC. The EUCAST antimycobacterial susceptibility testing subcommittee (AMST) compared protocols of MIC determination with regard to medium, inoculum preparation, antituberculous agent preparation, incubation, reading of the results and interpretation. The EUCAST reference method of MIC determination for MTBC is the broth microdilution method in Middlebrook 7H9-10% OADC medium. The final inoculum is a 105 CFU/mL suspension, obtained from a 10−2 dilution of a 0.5 McFarland suspension prepared after vortexing bacterial colonies with glass beads before suspending them in sterile water. The culture is maintained in a U-shaped 96-well polystyrene microtitre sterile plate with a lid incubated at 36° ± 1°C. Reading is done using an inverted mirror as soon as the 1:100 diluted control (i.e. 103 CFU/mL suspension) shows visual growth. The MIC, expressed in mg/L, is the lowest concentration that inhibits visual growth. Mycobacterium tuberculosis H37Rv ATCC 27294 is used as the reference strain and its targeted MIC values are within the range 0.03–0.12 for isoniazid, 0.12–0.5 for levofloxacin and 0.25–1 mg/L for amikacin. The EUCAST reference method for MTBC was endorsed by EUCAST after public consultation and will from now on be used to define EUCAST ECOFFs and clinical breakpoints. This reference method is not primarily intended to be used under routine conditions and the AST methods will need to be calibrated against this reference method to be used with EUCAST breakpoints. [ABSTRACT FROM AUTHOR]

Various methods have been developed to detect the presence of contamination with Coliforms and E. coli in foods. The pour plate technique using VRBA medium is confirmed as a standard method in Iran. The biggest disadvantage of thismethod is the need to spend a lot of time, high volume of laboratory operations, multiple stages and ultimately long time to achieve the results. Today, due to the mass productionof various foodstuffs, the need for faster methods with high sensitivity to control the quality of food is necessary for the responsible oversight centers. The use of chromogenic medias is also one of the fastest diagnostic methods that have been developed. According to this matter,a comparative study was considered from the results of application of three chromogenic media and reference method in food quality control. Totally 100 samples of foodstuffs were evaluated for contamination to Coliform and E.coli using standard method and three chromogenic medias. Based on the obtained results, 86, 79, 85 and 80 samples were contaminated to Coliform using the standard method, Coliform Agar ES, ChromAgar ECC and Rapid E.coli 2/Agar respectively. Also, using four mentioned methods, contamination to E.coli was reported at 66, 80, 84 and 80, respectively. Cochrane test showed that there was no significant difference between the four methods in Coliform diagnosis (p>0.05). However, four methods did not have the same function in the detection of E. coli so that the chromogenic methods showed significant difference with the standard method (p< 0/001). But there was no significant difference between these chromogenic methods in detecting E.coli (p>0.05). According to the statistical analysis of present study, three chromogenic medias can be used instead of the standard method for the detection of Coliform, but the use of these chromogenic medias is not recommended for the identification of E.coli. [ABSTRACT FROM AUTHOR]

Value addition of fresh tender jackfruit (Artocarpus heterophyllus L.) for vegetable purpose has gained much popularity due to its inherent nutritional and health benefits. For industries involved in value addition of tender jackfruit, rapid characterization of raw material is essential for screening and routine quality evaluation. But, conventional reference methods of quality evaluation are not suitable as they involve the use of chemicals, expensive, laborious and time consuming subject to the number of samples to be analyzed. As a promising alternative, the present study examined the performance of near-infrared spectroscopy (NIRS) as a novel approach to estimate pH, total soluble solid, titrable acidity, firmness and toughness of tender jackfruit. Partial least square regression (PLSR) models were used to establish linkage between reflectance spectra (1100-2450 nm) and quality attributes of fresh tender jackfruit. Based on residual prediction deviation (RPD) criteria, accuracy of PLSR model of titrable acidity was noted to be excellent (RPD=3.96) while good estimation was possible in case of firmness-tendril (RPD=2.61). Accuracy level suitable for coarse quantitative estimation (RPD=2.12) was noted in case of total soluble solids. The PLSR models of all other attributes were found to be capable of discriminating their low and high values (1.5

Accurate and precise cortisol measurements are requisite for ensuring appropriate diagnosis and management of diseases related with adrenal or pituitary gland disorders. Prompted by the needs in characterization of certified reference materials and quality assurance for serum cortisol measurements, we developed and evaluated a highly reliable measurement procedure based on isotope dilution liquid chromatography-tandem mass spectrometry (ID LC-MS/MS) combined with dextran sulfate-Mg2+ precipitation as the sample pretreatment. An appropriate amount of serum was accurately weighed and spiked with the isotope labelled internal standard. After precipitation, massive lipids and lipoproteins were removed from serum matrix. The clear supernatant was transferred and extracted with ethyl acetate-hexane solution. The cortisol was analyzed with LC-MS/MS in positive electrospray ionization mode. The within-run and total coefficient of variations (CVs) ranged from 0.3 to 0.6% and 0.7 to 1.2%, respectively, for a concentration range of 76.30 to 768.04 nmol/L. A regression comparison of the results obtained by the present method and the certified values of ERM-DA451 showed agreement with no statistical difference (Y = 1.0092 X-0.7455; 95% CI for the slope, 0.9940 to 1.0212; 95% CI for the intercept, − 3.6575 to 2.6390, r2 = 0.999). All structural analogs of cortisol tested were well resolved from cortisol in 12 min on a phenyl ligand column under an isocratic elution. The limit of quantification was estimated to 5 pg cortisol in absolute amount. This method is accurate and simple and can be served as a candidate reference measurement procedure in establishment of serum cortisol reference system. [ABSTRACT FROM AUTHOR]

Measurement of serum progesterone is important in determining ovarian function. Most progesterone measurements are performed with immunoassays and results are often variable. Standardization of the measurements requires a reliable reference method. An isotope dilution liquid chromatography tandem mass spectrometry (ID-LC/MS/MS) method for the measurement of serum progesterone was developed. Serum samples were spiked with 13C3-progesterone, extracted with a three-step liquid-liquid extraction, and analyzed by LC/MS/MS. A bracketing calibration was used for the analysis and samples were prepared gravimetrically. The developed method showed intra-run and total relative standard deviations (RSDs) of 0.50~0.58% and 0.71~1.33%, respectively. The analytical recoveries were 99.08~101.50%. Measurement results on certified reference materials obtained with this method agreed with the certified values within the stated measurement uncertainties. The method was applied to evaluate immunoassays through split-sample comparisons. A panel of 48 fresh frozen individual samples were measured with the ID-LC/MS/MS method, and six immunoassays and results were compared. Significant calibration biases and sample-specific deviations were observed on some of the immunoassays. [ABSTRACT FROM AUTHOR]

Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments, as well as for enforcing EU air quality regulations. Typically, airborne particles are sampled over long time periods on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). During the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling is combined for the first time with on-site total reflection X-ray fluorescence (TXRF) spectroscopy to develop a tool for quantifying particle element compositions within short time intervals and even on-site. This makes variations of aerosol chemistry observable with time resolution only a few hours and with good size resolution in the PM10 range. The study investigates the proof of principles of this methodological approach. Acrylic discs and silicon wafers are shown to be suitable impactor carriers with sufficiently smooth and clean surfaces, and a non-destructive elemental mass concentration measurement with a lower limit of detection around 10 pg/m3 could be achieved. We demonstrate the traceability of field TXRF measurements to a radiometrically calibrated TXRF reference, and the results from both analytical methods correspond satisfactorily.

A candidate reference measurement procedure (RMP) for measurement of unconjugated estriol in human serum has been developed and validated. The proposed method is highly reliable and uses isotope dilution coupled with liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) and requires no derivatization. An appropriate amount of serum was accurately weighed and spiked with an isotopically labeled internal standard. Unconjugated estriol and its internal standard were extracted from serum matrix using liquid-liquid extraction prior to reversed-phase LC-MS/MS. Calibrator bracketing was used to give higher specificity and accuracy for assigning serum level. The accuracy of the candidate RMP was validated by split-sample comparison to established RMPs. The lowest limit of detection (LLoD) and lowest limit of quantification (LLoQ) for developed RMP was estimated to be 0.14 nmol/L and 0.35 nmol/L, respectively. Both intra- and inter-assay imprecisions were ≤2.19% at 1.39, 17.34 and 69.35 nmol/L, respectively. Recoveries were 98.54% to 100.34% and linear response ranged from 0.35 to 173.38 nmol/L. No interference was observed. Biases were 5.6% and 2.8% against the targets of RELA2015A (3.87 nmol/L) and RELA2015B (40.62 nmol/L), respectively. Moreover, the candidate RMP was successfully applied to measure level of unconjugated estriol in serum samples of pregnant women (n = 3) and compared with two immunoassays in clinical laboratory. Our developed method is simple, accurate, and can be used as a candidate RMP to determine total unconjugated estriol level in human serum. Further improvement of certain immunoassays in accuracy and precision is needed.Selected ion chromatograms by LC-MS/MS using a C18 column for uE3 from a serum sample [ABSTRACT FROM AUTHOR]

The milk analyse result reliability is important for assurance of foodstuff chain quality. There are more direct and indirect methods for milk composition measurement (fat (F), protein (P), lactose (L) and solids non fat (SNF) content). The goal was to evaluate some reference and routine milk analytical procedures on result basis. The direct reference analyses were: F, fat content (Röse–Gottlieb method); P, crude protein content (Kjeldahl method); L, lactose (monohydrate, polarimetric method); SNF, solids non fat (gravimetric method). F, P, L and SNF were determined also by various indirect methods: – MIR (infrared (IR) technology with optical filters), 7 instruments in 4 labs; – MIR–FT (IR spectroscopy with Fourier’s transformations), 10 in 6; – ultrasonic method (UM), 3 in 1; – analysis by the blue and red box (BRB), 1 v 1. There were used 10 reference milk samples. Coefficient of determination (R2), correlation coefficient (r) and standard deviation of the mean of individual differences (MDsd, for n) were evaluated. All correlations (r; for all indirect and alternative methods and all milk components) were significant (P ≤ 0.001). MIR and MIR–FT (conventional) methods explained considerably higher proportion of the variability in reference results than the UM and BRB methods (alternative). All r average values (x minus 1.64 × sd for 95% confidence interval) can be used as standards for calibration quality evaluation (MIR, MIR–FT, UM and BRB): – for F 0.997, 0.997, 0.99 and 0.995; – for P 0.986, 0.981, 0.828 and 0.864; – for L 0.968, 0.871, 0.705 and 0.761; – for SNF 0.992, 0.993, 0.911 and 0.872. Similarly ​MDsd (x plus 1.64 × sd): – for F 0.071, 0.068, 0.132 and 0.101%; – for P 0.051, 0.054, 0.202 and 0.14%; – for L 0.037, 0.074, 0.113 and 0.11%; – for SNF 0.052, 0.068, 0.141 and 0.204.

Blood-based indicators that are used in the assessment of iron status are assumed to be accurate. In practice, inaccuracies in these measurements exist and stem from bias and variability. For example, the analytic variability of serum ferritin measurements across laboratories is very high (≥15%), which increases the rate of misclassification in clinical and epidemiologic studies. The procedures that are used in laboratory medicine to minimize bias and variability could be used effectively in clinical research studies, particularly in the evaluation of iron deficiency and its associated anemia in pregnancy and early childhood and in characterizing states of iron repletion and excess. The harmonization and standardization of traditional and novel bioindicators of iron status will allow results from clinical studies to be more meaningfully translated into clinical practice by providing a firm foundation for clinical laboratories to set appropriate cutoffs. In addition, proficiency testing monitors the performance of the methods over time. It is important that measures of iron status be evaluated, validated, and performed in a manner that is consistent with standard procedures in laboratory medicine. [ABSTRACT FROM AUTHOR]

The total haemoglobin (Hb) concentration in blood is one of the most frequently measured analytes in clinical medicine because of its significance for evaluating the health state of a human. The spectrophotometric cyanmethaemoglobin (HiCN) method is the internationally accepted conventional reference method to determine this biomarker. It is frequently used in clinical routine diagnostics but is not traceable to the International System of Units and thus does not meet highest metrological demands. A further critical issue is the toxicity of the necessary potassium cyanide. Different methods to solve these problems are reported here. They all were validated against the HiCN method in an interlaboratory comparison by measuring the total Hb concentration present in the certified reference material JCCRM 912-2M. Methods considered were the spectrophotometric alkaline haematin detergent (AHD) method as well as several isotope dilution (ID)-based approaches. The latter include inductively coupled plasma mass spectrometry (ICP-MS), species-specific (SS) ICP-MS, organic MS and Raman spectrometry. [ABSTRACT FROM AUTHOR]

Wastewater analysis is an important area in analytical and environmental chemistry. It can be performed with both the classic wet methods and instrumental techniques. The development of new methods, and modification of the existing ones, constitute a major task for researchers. Ion chromatography plays a predominant role in ion determinations with the instrumental methods. It offers several advantages over the conventional methods, such as simultaneous determinations of alkali and alkaline earth cations and ammonia. Ammonium ions cannot be determined by spectroscopic methods. Ion chromatography has been accepted world-wide as a reference method for analyzing anions and cations in water and wastewater due to the fact that it enables the replacement of several individual wet chemistry methods for common ions with one instrumental technique. The following article describes the principles of ion chromatography, such as stationary phases, eluents, detectors, and sample preparation methods. Moreover, the applications of ion chromatography in wastewater analyses and international standards are presented.

Casein measurement is important for cheesemaking and control of dairy cow nutrition. Reference Kjeldahl method is not suitable for routine purposes. Infra-red spectroscopy MIR and MIR-FT use can be a solutin. However, their casein specifity is relatively limited. Aim of the work was to assess the quality of performed calibrations for validation of calibration parameters. A retrospective analysis of MIR and MIR-FT calibrations was performed for estimation of limits their suitable parameters. Mean casein values of reference sample sets varied from 2.49 to 2.7% (2.61 ± 0.155). Mean variation range was 0.561 ± 0.164%. The mean correlation coefficient of calibration (KKK) was 0.974 ± 0.018 (P < 0.001). The mean standard deviation of mean for individual differences (SDID) was 0.03 ± 0.011% (from 0.01 to 0.08). MIR-FT results were slightly better both for calibration and for proficiency testing. The high and low KKKs were higher in the case of accepted calibration as in proficiency testing for MIR-FT and MIR (0.986 > 0.964 and 0.970 > 0.948; 0.982 > 0.947 and 0.947 > 0.911; P < 0.001). The casein number varied from 79.4 to 80.56% in bulk milk samples in three years, its variability was low from 1.4 to 1.5% relatively, which shows on relatively reliable casein analyses by methods MIR and MIR-FT. It does not need to agree fuly for individual milk samples. It is linked more to MIR than MIR-FT. Limits for acceptable calibration parameters were derived: > 0.945 for KKK; 0.048 for SDID and 0.029% for mean difference as maximum.

Important objectives of External Quality Assessment (EQA) is to detect analytical errors and make corrective actions. The aim of this paper is to describe knowledge required to interpret EQA results and present a structured approach on how to handle deviating EQA results. The value of EQA and how the EQA result should be interpreted depends on five key points: the control material, the target value, the number of replicates, the acceptance limits and between lot variations in reagents used in measurement procedures. This will also affect the process of finding the sources of errors when they appear. The ideal EQA sample has two important properties: it behaves as a native patient sample in all methods (is commutable) and has a target value established with a reference method. If either of these two criteria is not entirely fulfilled, results not related to the performance of the laboratory may arise. To help and guide the laboratories in handling a deviating EQA result, the Norwegian Clinical Chemistry EQA Program (NKK) has developed a flowchart with additional comments that could be used by the laboratories e.g. in their quality system, to document action against deviations in EQA. This EQA-based trouble-shooting tool has been developed further in cooperation with the External quality Control for Assays and Tests (ECAT) Foundation. This flowchart will become available in a public domain, i.e. the website of the European organisation for External Quality Assurance Providers in Laboratory Medicine (EQALM). [ABSTRACT FROM AUTHOR]

Non-structural carbohydrates (NSC) in plant tissue are frequently quantified to make inferences about plant responses to environmental conditions. Laboratories publishing estimates of NSC of woody plants use many different methods to evaluate NSC. We asked whether NSC estimates in the recent literature could be quantitatively compared among studies. We also asked whether any differences among laboratories were related to the extraction and quantification methods used to determine starch and sugar concentrations. These questions were addressed by sending sub-samples collected from five woody plant tissues, which varied in NSC content and chemical composition, to 29 laboratories. Each laboratory analyzed the samples with their laboratory-specific protocols, based on recent publications, to determine concentrations of soluble sugars, starch and their sum, total NSC. Laboratory estimates differed substantially for all samples. For example, estimates for Eucalyptus globulus leaves (EGL) varied from 23 to 116 (mean = 56) mg g-1 for soluble sugars, 6-533 (mean = 94) mg g-1 for starch and 53-649 (mean = 153) mg g-1 for total NSC. Mixed model analysis of variance showed that much of the variability among laboratories was unrelated to the categories we used for extraction and quantification methods (method category R² = 0.05-0.12 for soluble sugars, 0.10-0.33 for starch and 0.01-0.09 for total NSC). For EGL, the difference between the highest and lowest least squares means for categories in the mixed model analysis was 33 mg g-1 for total NSC, compared with the range of laboratory estimates of 596 mg g-1. Laboratories were reasonably consistent in their ranks of estimates among tissues for starch (r = 0.41-0.91), but less so for total NSC (r = 0.45-0.84) and soluble sugars (r = 0.11-0.83). Our results show that NSC estimates for woody plant tissues cannot be compared among laboratories. The relative changes in NSC between treatments measured within a laboratory may be comparable within and between laboratories, especially for starch. To obtain comparable NSC estimates, we suggest that users can either adopt the reference method given in this publication, or report estimates for a portion of samples using the reference method, and report estimates for a standard reference material. Researchers interested in NSC estimates should work to identify and adopt standard methods. [ABSTRACT FROM AUTHOR]

The inaccuracy of routine serum 25-hydroxyvitamin D measurements hampers the interpretation of data in patient care and public health research. We developed and validated a candidate reference measurement procedure (RMP) for highly accurate quantitation of two clinically important 25-hydroxyvitamin D metabolites in serum, 25-hydroxyvitamin D [25(OH)D] and 25-hydroxyvitamin D [25(OH)D]. The two compounds of interest together with spiked deuterium-labeled internal standards [ d-25(OH)D and d-25(OH)D] were extracted from serum via liquid-liquid extraction. The featured isotope-dilution LC-MS/MS method used reversed-phase chromatography and atmospheric pressure chemical ionization in positive ion mode. A pentafluorophenylpropyl-packed UHPLC column together with isocratic elution allowed for complete baseline resolution of 25(OH)D and 25(OH)D from their structural C-3 isomers within 12 min. We evaluated method trueness, precision, potential interferences, matrix effects, limits of quantitation, and measurement uncertainty. Calibration materials were, or were traceable to, NIST Standard Reference Materials 2972. Within-day and total imprecision (CV) averaged 1.9 and 2.0 % for 25(OH)D, respectively, and 2.4 and 3.5 % for 25(OH)D, respectively. Mean trueness was 100.3 % for 25(OH)D and 25(OH)D. The limits of quantitation/limits of detection were 4.61/1.38 nmol/L for 25(OH)D and 1.46/0.13 nmol/L for 25(OH)D. When we compared our RMP results to an established RMP using 40 serum samples, we found a nonsignificant mean bias of 0.2 % for total 25(OH)D. This candidate RMP for 25(OH)D metabolites meets predefined method performance specifications (≤5 % total CV and ≤1.7 % bias) and provides sufficient sample throughput to meet the needs of the Centers for Disease Control and Prevention Vitamin D Standardization Certification Program. [Figure not available: see fulltext.] [ABSTRACT FROM AUTHOR]

Objectives: The aim of the current study was to establish a reliable candidate reference method for serum 25-hydroxyvitamin D [25(OH)D] measurement and to assess the commutability of multiple control materials among liquid chromatography-tandem mass spectrometry (LC-MS/MS) methods., Methods: Serum 25-hydroxyvitamin D2 [25(OH)D2] and 25-hydroxyvitamin D3 [25(OH)D3] together with spiked internal standards were extracted with a one-step approach and then analyzed by LC-MS/MS. The commutability assessment for 25(OH)D was conducted according to the Clinical and Laboratory Standards Institute (CLSI) EP14-A3 protocol. 25(OH)D concentrations in 5 levels of unprocessed serum pools, 7 levels of serum pools spiked with 25(OH)D3 or 25(OH)D2, 3 levels of commercial control materials, 2 levels of spiked bovine serum, and 4 levels of external quality assessment (EQA) materials were measured along with 30 single-donor samples using the candidate reference method and two routine LC-MS/MS methods., Results: The candidate reference method could separate 25(OH)D2 and 25(OH)D3 from 14 potential interfering compounds completely within a 9-min analysis time. Good method precision was obtained, and measurement results on certified reference material NIST SRM 972a were within the uncertainty of the certified values. All candidate materials were assessed commutable for LC-MS/MS methods., Conclusions: The candidate reference method for serum 25(OH)D measurement is precise, accurate, and robust against interferences and can provide an accuracy base for routine methods. The multiple alternative control materials with commutability among LC-MS/MS methods will facilitate the further standardization for serum 25(OH)D measurement., (© 2022 The Authors. Journal of Clinical Laboratory Analysis published by Wiley Periodicals LLC.)

Most of the reflectometry methods which are used for determining the phase of complex reflection coefficient such as reference method and Variation of Surroundings medium are based on solving the Schrödinger equation using a discontinuous and step-like scattering optical potential. However, during the deposition process for making a real sample the two adjacent layers are mixed together and the interface would not be discontinuous and sharp. The smearing of adjacent layers at the interface (smoothness of interface), would affect the reflectivity, phase of reflection coefficient and reconstruction of the scattering length density (SLD) of the sample. In this paper, we have investigated the stability of reference method in the presence of smooth interfaces. The smoothness of interfaces is considered by using a continuous function scattering potential. We have also proposed a method to achieve the most reliable output result while retrieving the SLD of the sample. [ABSTRACT FROM AUTHOR]

We propose isotope-dilution mass spectrometry as a candidate reference method for determination of serum cortisol. The method uses liquid chromatography-mass spectrometry (LC-MS), interfaced with electrospray ionization, and selective monitoring of the [M+H]+ ions of cortisol and isotopically labeled cortisol. The isotope-dilution-liquid chromatography-mass spectrometry (ID-LC-MS) method simplifies sample-preparation, because samples are processed by simple solvent extraction without further clean-up and derivatization. We studied the time required for complete equilibration of endogenous cortisol and labeled cortisol spiked into serum and found it to be less than 1 h. The repeatability and the reproducibility of the method were evaluated and found to be 0.55% of the measurement value. CRM 192 and 193 from the Bureau Communautaire de Reference were analyzed for verification of the method. The results obtained from the ID-LC-MS method agreed with the certified values. The relative uncertainty of measurement results for samples in the range of a few tens of micrograms per kilogram to several hundred micrograms per kilogram was evaluated and found to be 0.56%. Immunoassay carried out by three independent clinical laboratories produced results more than 15% higher than this ID-LC-MS method, suggesting the presence of bias in the immunoassay methods. [ABSTRACT FROM AUTHOR]

Most of the reflectometry methods which are used for determining the phase of complex reflection coefficient such as Reference Method and Variation of Surroundings medium are based on solving the Schrödinger equation using a discontinuous and step-like scattering optical potential. However, during the deposition process for making a real sample the two adjacent layers are mixed together and the interface would not be discontinuous and sharp. The smearing of adjacent layers at the interface (smoothness of interface), would affect the the reflectivity, phase of reflection coefficient and reconstruction of the scattering length density (SLD) of the sample. In this paper, we have investigated the stability of Reference Method in the presence of smooth interfaces. The smoothness of interfaces is considered by using a continuous function scattering potential. We have also proposed a method to achieve the most reliable output result while retrieving the SLD of the sample.

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To compare fosfomycin susceptibility testing with the commercial agar dilution (AD) test, AD Fosfomycin (Liofilchem, Roseto degli Abruzzi, Italy) and the reference AD method, using a collection of multidrug-resistant (MDR) Enterobacterales and Pseudomonas aeruginosa clinical isolates. The collection included 119 carbapenemase-producing Enterobacterales , 53 Enterobacterales producing acquired AmpC-type and/or extended-spectrum β-lactamases and 38 carbapenemase-producing P. aeruginosa , including representatives of different high-risk clones. AD Fosfomycin and AD reference method (ISO 20776-1:2019) were performed starting from the same microbial suspension. Results were interpreted according to EUCAST clinical breakpoints (10.0). Essential agreement (EA), category agreement (CA) and error rates were calculated as described by the International Organization for Standardization. Of 172 Enterobacterales, 143 (83.1%, including 92.9% (52 of 56) of the NDM-producers and 84.2% (48 of 57) of the KPC-producers) were susceptible to fosfomycin using reference AD. A CA of 91.9% (158 of 172; 95% CI 87.1%–95.3%) and an EA of 92.5% (136 of 147; 95% CI 87.4%–96.0%), respectively, were calculated for the commercial AD Fosfomycin test, with 9.8% (14 of 143) of major errors and no very major errors (0 of 29). Overall, 86.8% (33 of 38) of P. aeruginosa showed a fosfomycin MIC ≤128 mg/L using reference AD. An EA of 84.8% (95% CI 66.3%–92.0%) was calculated for the commercial AD Fosfomycin test, with a CA of 100% (95% CI 93.6%–100%) when considering a tentative breakpoint at 128 mg/L. AD Fosfomycin showed an overall good concordance compared with reference AD. [ABSTRACT FROM AUTHOR]

Quantitative chemical analysis of airborne particulate matter (PM) is vital for the understanding of health effects in indoor and outdoor environments, as well as for enforcing EU air quality regulations. Typically, airborne particles are sampled over long time periods on filters, followed by lab-based analysis, e.g., with inductively coupled plasma mass spectrometry (ICP-MS). During the EURAMET EMPIR AEROMET project, cascade impactor aerosol sampling is combined for the first time with on-site total reflection X-ray fluorescence (TXRF) spectroscopy to develop a tool for quantifying particle element compositions within short time intervals and even on-site. This makes variations of aerosol chemistry observable with time resolution only a few hours and with good size resolution in the PM10 range. The study investigates the proof of principles of this methodological approach. Acrylic discs and silicon wafers are shown to be suitable impactor carriers with sufficiently smooth and clean surfaces, and a non-destructive elemental mass concentration measurement with a lower limit of detection around 10 pg/m3 could be achieved. We demonstrate the traceability of field TXRF measurements to a radiometrically calibrated TXRF reference, and the results from both analytical methods correspond satisfactorily. [ABSTRACT FROM AUTHOR]