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A rapid, sensitive, specific, accurate and precise high pressure liquid chromatographic method (HPLC) method involving UV detection has been developed for the determination and quantification of Amlodipine Besylate and Enalapril maleate in bulk and combined dosage form. The determination was carried out on a Phenomenex C18 column (Dimention : 250 x 4.6 mm, 5 ?m). The sample was analysed using filtered and degassed mixture of methanol : 0.1N HCl (1:1) as mobile phase at a flow rate of 1ml/min and effluent was monitored at 218nm. The retention time for Amlodipine besylate was 7.6 min and for Enalapril maleate 3.2 min. Amlodipine besylate and Enalapril maleate showed a linear response in the concentration range of 10-50?g/ml. The correlation co-efficient ('r' value) for Amlodipine besylate and Enalapril maleate was 0.9992 and 0.9994, respectively. The method was validated in terms of linearity, precision, accuracy, specificity, robustness and solution stability. The proposed method can be used for routine analysis of Amlodipine Besylate and Enalapril maleate in bulk and combined dosage form Keywords: Amlodipine besylate, Enalapril maleate, Method development, Validation, HPLC

The objective of this experiment was to develop and validate a simple, robust, and accurate QbD based Reverse-Phase High-Performance Liquid Chromatography method for Simultaneous estimation of Amlodipine besylate and Lisinopril dihydrate in bulk and Pharmaceutical Dosage form. A box-Behnken design was employed for optimizing the mobile phase, flow rate and pH of buffer, the optimized chromatographic conditions were Phosphate buffer: Methanol (25: 75 v/v), pH of buffer: 6.5 and flow rate: 1mL/min. Furthermore formulation injected and observed that the additives do not interfere with the peak of Amlodipine besylate and Lisinopril dehydrate. Both drugs are well resolved and Retention times were found to be 2.332 min and 3.584 min respectively. Linearity was observed in the concentration range of 10 μg to 50 μg/mL (r2=0.999). The accuracy range was 99.75 to 100.04%. Intra-day and Inter-day precision was found to be less than 2% RSD. The proposed method was useful for the best analysis of Amlodipine besylate and Lisinopril dihydrate in Bulk, pharmaceutical dosage forms and was successfully applied to routine analysis.

Background Rebamipide (REB) is quinolinone derivative compound, which is used for the treatment of stomach ulcers. Objective The development of four spectrophotometric methods for quantification of REB and its impurity and degradation product: the debenzoylated isomer of REB (DER). Methods Method A is ratio difference spectrophotometry where 254 and 291 nm were selected for REB and 320 and 355 nm were selected for DER, allowing spectral discrimination for both. Method B is derivative ratio spectrophotometry, where the peak amplitudes of the first derivative of ratio spectra at 261 and 350.2 nm for REB and DER, respectively, are determined. Method C is a second derivative approach, which allows quantification of both REB and DER at 337 and 340 nm, respectively. Method D is mean centering of ratio spectra, where electronic absorption spectra of REB and DER were recorded and divided by a suitable divisor from DER and REB, respectively, and then the mean center is represented by the ratio spectrum so obtained. Results The proposed methods are simple, selective, and sensitive in the quantification of REB and DER. These methods were validated according to International Conference on Harmonization guidelines. Statistical analyses performed on the findings from the suggested methods and those obtained from reported methods revealed high accuracy and good precision. Conclusion The developed and validated methods are useful for quality control assay in routine analyses. Highlights First derivative, second derivative, derivative ratio, and mean centering methods for quantification of REM and DER. These methods are useful for analysis of REB in pharmaceutical dosage form.

A high-performance thin-layer chromatography (HPTLC) method has been developed for the quantitative determination and validation of plumbagin in the methanolic fraction of Plumbago zeylanica. For achieving good separation, the mobile phase of toluene‒ethyl acetate (9:2, V/V) for plumbagin was used. Densitometric determination of plumbagin was carried out at 270 nm in reflection/absorption mode; the calibration curves were linear in the range of 100‒600 ng/spot. During analysis, the methanolic fraction of P. zeylanica L. showed the presence of plumbagin. The method is specific, simple, precise, and accurate. The obtained data can be used for the routine analysis of the reported biomarkers in crude drugs and extracts. The quantification and the method validation of these biomarkers have not yet been reported in P. zeylanica which can be utilized for the proper standardization of the plant.

Background In the present study, an HPTLC (high-performance thin-layer chromatography) method was developed for the quantitative determination and validation of the curcumin in the methanolic fraction of Curcuma longa L. For achieving good separation of curcumin, the mobile phase of chloroform:methanol (97:3) was used. The densitometric analysis of curcumin was performed at 420 nm in reflection/absorption mode. Results Linearity of the method was obtained in the range of 100‒600 ng per spot. During analysis, the methanolic fraction of the C. longa showed the presence of a quantifiable amount of curcumin. The content of curcumin was found to be 1.5% (per dry weight). Conclusions The method is specific, simple, precise, and accurate. The obtained data can have used for the routine analysis of the reported biomarkers in crude drugs and extracts. The quantification and the method validation of curcumin have not yet been reported in C. longa which can be utilized for the proper standardization of the plant.

Background The green chemistry approach was developed for the purpose of saving the environment by using green solvents. Applying green analytical chemistry principles to traditional methods is considered a challenge. Acemetacin is a commonly used analgesic prodrug that bioactivates to indomethacin. Objective Developing two simple, eco-friendly chromatographic methods for simultaneous determination of acemetacin and indomethacin. Method The first method is HPLC-DAD. Separation was performed on a Waters XBridge® Shield RP18 (250 × 4.6 mm, 5 µm) analytical column with ethanol–ammonium acetate buffer (50 mM, pH 3.5 ± 0.1; 60:40, v/v) as a mobile phase at a flow rate of 1 mL/min at 25 ± 0.5°C and UV detection at 254 nm. The other method is TLC coupled with densitometric quantification using pre-coated silica TLC plates and butanol–ethyl acetate (70:30, v/v) elution system. The plates were scanned at 254 nm. Results Both methods were validated according to International Conference on Harmonization guidelines. Linearity was confirmed for both over a concentration range of 1–100 µg/mL for the HPLC method and 0.2–7 µg/band for TLC-densitometric method. The methods’ greenness was evaluated by the National Environmental Methods Index, Eco-Scale, Green Analytical Procedure Index metrics and Analytical GREEnness Metric Approach. Conclusions The proposed methods were found to be suitable for determination of studied drugs in their marketed formulations and is suggested for routine analysis in quality control laboratories. Highlights The developed HPLC method shortened the elution time of the analyzed drugs saving more time and money and the TLC method lowered the drugs’ detection limit. HPLC and TLC methods were validated for the assay of acemetacin and indomethacin. The methods’ greenness was evaluated and compared to published methods. The developed HPLC method shortened the elution time of the analyzed drugs, saving time and money and the TLC method lowered the drugs’ detection limit.

Indtroduction and methods: In chronic lymphocytic leukemia (CLL), molecular and cytogenetic diagnostics are crucial for the determination of accurate prognosis and treatment choice. Among different genetic aberrations, del(17p13) or TP53 mutations constitute high-risk factors, and early identification of such defects is a high priority for CLL patients. While cytogenetic diagnostics is well-established and accessible for the majority of CLL patients in Poland, molecular diagnostics of TP53 mutations is performed only in a few ERIC-certified centers (eight as of September 2020), and only two of these employ next-generation sequencing (NGS) for routine analysis of TP53 status in CLL patients. Here we report the interim results of a project assessing TP53 mutations with NGS technology in relapsed or refractory CLL patients with confirmed negative del(17p13) status. 249 patients from 32 clinical centers were included in the study. Results: NGS analysis revealed TP53 mutations in 42/249 (17%) patients, half of whom (21/249, 8.5%) had subclonal mutations (VAF ≤10%). These results are in line with published data in relapsed/refractory CLL patients. Conclusions: The results of the project demonstrated the feasibility and accuracy of NGS testing in CLL patients despite several initial logistical and technical obstacles. Our study also proved that, with appropriate funding, CLL patients from any hematological center in Poland can have access to state-of-the-art molecular diagnostics

The routine analysis of low molecular weight analytes by mass spectrometry is often complicated by the lability of the analyte’s functional groups and/or the lack of moieties that can be easily charged. If a molecule is too labile this precludes analysis by techniques such as electron ionisation or chemical ionisation as the analyte will undergo thermal decomposition prior to ionisation as well as spontaneous fragmentation during the ionisation process. If the analyte has a low propensity to form ions in electrospray ionisation (i.e., lacks acidic or basic sites) then often no analyte related ions are observed. In this paper, the robustness and versatility of the established method of atmospheric pressure chemical ionisation is demonstrated for the analysis of low molecular weight analytes. The utility of the technique is demonstrated through the analysis of 30 reference standards of varying functionality, and further by the analysis of 75 synthetic samples which were problematic when analysed by electron or electrospray ionisation. The resulting spectra are dominated by intact molecular species ([M+H]+ and M+ in positive ion mode and [M − H]− and [M + Cl]− in negative ion mode) along with logical neutral losses reminiscent of what you might expect from the analyte’s structure (losses of H2O from alcohols or CO from aldehydes etc). This paper presents atmospheric pressure chemical ionisation as an essential tool for broadening the chemical space of successful analyses for any routine mass spectrometry service laboratory of facility.

The field of agriculture is the key role in Indian society in which insecticides play a vital role in increasing the crop production yield. Carbosulfan is a member of the carbamate family; it is an important insecticide and it has a diversified role in agriculture. There is an increasing number of human poisoning cases by mainly the compound carbosulfan of the carbamate family. During the last few years, Forensic Science Laboratories of Maharashtra, India, detected a large number of human poisoning cases with carbosulfan since a large number of biological samples (postmortem sample) were received for toxicological chemical analysis. Thin-layer chromatography (TLC) and high-performance thin-layer chromatography (HPTLC) were the preferred methods of choice. By observing the results of toxicological chemical analysis, the conclusion can be drawn that carbosulfan plays a major role in poisoning cases. The chromogenic reagent was found to be a selective spray reagent for carbosulfan in routine analysis by HPTLC. Carbosulfan reacts with chromogenic reagent which gives more intense pink-colored compounds than the other organochlorine insecticides, organophosphorus insecticides, and pyrethroid insecticides. Biological material constituents (amino acids, peptides, proteins, fats, etc.) do not interfere with this chromogenic reagent.

Background Rice plays a significant role in providing basic energy and essential nutrients for humans. Its quality is of great concern to the agricultural industries and consumers. Due to the changes of external storage conditions and its own enzyme activity, rice undergoes the aging process, thus significantly decreasing its quality. Consequently, the development of a rapid, non-destructive, real-time detection method for rice quality inspection is urgently needed. Scope and approach In this article, the characteristics of volatile organic compounds (VOCs) that greatly contribute to aroma profiles of rice are introduced. Meanwhile, the working principles and applications of an electronic nose (E-nose) device as a reliable measurement in rice quality assessment based on the variation of aroma profiles are highlighted. Furthermore, comparisons between E-nose and traditional instrumental assessment methods, such as sensory evaluation, physical and chemical indicators, instrumental analysis, are made. In addition, this article also offers an insight into the challenges and future trends of the application of E-nose for rice quality inspection. Key findings and conclusion 2-acetyl-1-pyrroline (2-AP), aldehydes, heterocycles and alcohols have been identified as the major VOCs in rice aging. Through the comparison between E-nose and traditional instrumental measurements, E-nose has a huge potential for the rapid inspection of rice quality as it has numerous advantages in routine analysis. Furthermore, reducing the working temperature, utilizing appropriate pattern recognition methods and establishing new prediction models should be the future trends of E-nose employed as an effective detection method in rice quality inspection.

A simple, accurate and precise RP-HPLC method was developed for the simultaneous determination of chloroquine, pyrimethamine and cetirizine hydrochloride concentrations in bulk drug and human serum. The assay was performed using a mobile phase of methanol: water (70:30) at pH of 2.8 ± 0.05 on the Purospher C-18 column with UV detection at 230 nm and rosuvastatin used as an internal standard. The retention times observed for chloroquine, pyrimethamine and cetirizine hydrochloride were 3.5, 2.5 and 5.5 minutes, respectively. The method was found to be specific for the assayed drugs showing a linear response in the concentration range of 1–100 μg mL−1 with coefficients of determination values of (r = 0.999). The method was developed and validated according to ICH guidelines. The method was used to monitor the serum samples and was found to be sensitive for therapeutic purposes, showing the potential to be a useful tool for routine analysis in laboratories.

A multiresidue method without cleanup step was validated for simultaneous determination of multiclass pesticide residues in rice. The extracted incurred residues of pesticides were separated on a reversed-phase column and quantified by tandem mass spectrometry (MS/MS). The method accuracy was in the range of 71–108%, and the precision was in the range of 4–20% for 25 out of 28 selected pesticides. The method quantification limits for 25 selected pesticides were below Codex and EU maximum residue limits (MRL). The selected 25 pesticides met the EU-SANTE and FAO/WHO Codex Alimentarius Commission method validation guidelines. The interday repeatability of the optimized method was between 4 and 18% (n = 6). The expanded uncertainty calculated for the optimized method ranged from 22 to 48%. The results obtained demonstrated the method's suitability for routine analysis. In total, 35 samples were analyzed of which, 22 samples (62%) were found to be contaminated with pesticides concentrations ranging from 0.010 to 0.297 mgkg−1.

The high-performance liquid chromatography-mass spectrometry (LC-MS) technique is widely applied to routine analysis in many matrices. Despite the enormous application of LC/MS, this technique is subjected to drawbacks called matrix effects (MEs) that could lead to ion suppression or ion enhancement. This phenomenon can exert a deleterious impact on the ionization efficacy of an analyte and subsequently on the important method performance parameters. LC-MS susceptibility to MEs is the main challenge of this technique in the analysis of complex matrices such as biological and food samples. Nowadays, the assessment, estimation, and overcoming of the MEs before developing a method is mandatory in any analysis. Two main approaches including the post-column infusion and post-extraction spike are proposed to determine the degree of MEs. Different strategies can be adopted to reduce or eliminate MEs depending on the complexity of the matrix. This could be done by improving extraction and clean-up methods, changing the type of ionization employed, optimization of liquid chromatography conditions, and using corrective calibration methods. This review article will provide an overview of the MEs as the Achilles heel of the LC-MS technique, the causes of ME occurrence, their consequences, and systemic approaches towards overcoming MEs during LC-MS-based multi-analyte procedures.

Dexamethasone sodium phosphate (DSP) is an ester of dexamethasone with anti-inflammatory action. This study provides new insights to develop a simple, precise, and accurate spectrophotometric method for the quantitative determination of DSP in bulk and pharmaceuticals. The method was validated before being applied to determine the DSP in six pharmaceutical injection forms from different companies. DSP is soluble in phosphate buffer, so it was used as a solvent, and a pH of 6 was found to be suitable for determination purposes. The DSP solution was scanned in the ultraviolet range (200–400 nm) using a double-beam spectrophotometer with a 1-cm quartz cell. The wavelength (λ max) of DSP was set at 242.5 nm, following the Beer–Lambert law for concentrations from 2 to 50 μg/ml. Dexa AIWA (Germany) showed the best results, being very close to the bulk value with no significant variation. Similarly, Dexamed (Cyprus) and HEMAZON (Syria) showed no significant differences from the bulk; however, the three remaining injections, DEXAKAL (India), DEXABRU (India), and DEXARON (China), showed significant variations from the bulk. Estimated limit of detection and limit of quantitation values for DSP were 0.83 and 2.5 μg/ml, respectively, with a regression coefficient of 0.999. Recovery studies were then used to determine the accuracy of the suggested method. The percentage of recovery was found to be 98.58%–102.52%. All results are suggesting a pivotal method for the routine analysis of DSP both in pure form and the commercially pharmaceutical forms.

Introduction The quantitation of glucagon remains a challenging immunoassay, mainly due to cross-reactivity. A sensitive, rapid and specific intact glucagon method is therefore necessary for quality routine analysis. A tandem mass spectrometry method to fulfill this objective is described in this work. Methods Glucagon was extracted from plasma employing a mixed-mode anion exchange solid-phase extraction. Sample stability was assessed in K2-EDTA and P800 tubes at different temperatures. We compared our method to two different immunoassays. FDA and EMA guidelines were followed for validation. An external quality control program served for comparison with other laboratories. Results Assay imprecision was below 4%. Recoveries were within 95–103%. LoQ was 8.75 pg/mL. Total analytical CV was 2.91%. Samples were found stable at 4 °C for less than 4 h. Diasource® RIA disagreed with our method. Mercodia® ELISA provided a closer agreement, also proven by external quality control samples. Conclusions A rapid and specific LC-MS/MS method for glucagon quantitation has been developed, validated and is suitable to routine care. The simplicity and the good performances in terms of time and specificity, could open the possibility to establish a standardized method for glucagon.

The combination of Canagliflozin and Metformin was available as fixed dose tablets for the treatment of type 2 diabetes. The present method aims to develop a simple, precise and accurate spectrophotometric method for simultaneous determination of Canagliflozin and Metformin in commercial formulation. The method utilizes Vierordt’s equation based on the measurement at two wavelengths 290nm (?max of Canagliflozin) and 236nm (?max of Metformin). The method exhibited linear range of 2.5 to 15µg/ml and 5 to 17.5µg/ml for Canagliflozin and Metformin, respectively, with a correlation coefficient of 0.999. The LOD and LOQ for Canagliflozin were found to be 0.43 and 1.31 respectively. For Metformin the LOD and LOQ were found to be 0.49 and 1.49 respectively. The recovery of Canagliflozin and Metformin were found to be 99.43 and 98.82 respectively. The results were validated statistically as per ICH guidelines and were found to be satisfactory. To conclude, the developed UV spectrophotometric method is more economical for analysis of Canagliflozin and Metformin in both bulk and pharmaceutical dosage form for routine analysis. Keywords: Canagliflozin, Metformin, Vierordt’s equation, UV-Spectrophotometry, ICH guidelines

Aims: To quantify pamidronate in a sensitive and accurate way either in bulk or dosage forms. Methodology: The quantification of this group of drugs is a challenging task as they lack the presence of chromophore groups in their structure. The proposed method depends on the derivatization of the studied drug by its reaction with 4-Chloro-7-nitro-2,1,3-benzoxazole and the product is measured spectrophotometrically at 470 nm. The conditions for the reaction are optimized regarding the volume of the reagent, the optimum pH for the reaction completion, the buffer volume, the optimum temperature for the reaction and the optimum heating time. Results: The studied drug can be determined in the range of 9-30 µg/mL after optimizing the reaction conditions. Method validation is performed according to ICH guidelines and different validation parameters like, linearity, accuracy, precision and robustness are calculated and found to be excellent. Conclusion: The proposed method is accurate, sensitive and can be applied for the routine analysis of pamidronate in quality control laboratories.

The purpose of present effort was to conduct physiochemical evaluation of miscellaneous commercially available diclofenac potassium 75 mg tablets in the local market of Sindh, Pakistan. Further comparison was made among their different parameters. In study seven brands tagged as RB1 to RB7 were evaluated for diameter, thickness, disintegration time, and assay content and dissolution profile. Obtained results of all brands conformed to the official standard specification for disintegration test, Assay Content. The attained release rate profile during dissolution study revealed that all brands achieved more than 80% in sixty minutes. The spectrophotometric analysis for assay content of all brands was within 90%-110% which in good agreement with specified in the Unites States Pharmacopoeia. In the current study all the assessed products could be regarded as being chemically similar, while no product is found as a false product, these all brands can be used alternatively. The used spectrophotometric evaluation is very simple, reasonable, and easy to adopt for analysis and could be used in routine analysis of diclofenac potassium tablets, particularly in the unavailability of advanced equipment’s just like HPLC, LCMS & GC etc. which is not easily available and accusable in many institutions.

A simple and selective LC technique is chosen for the determination of Aceclofenac and Tizanidine in pill indefinite quantity forms. Chromatographic process separation was achieved on a c18 column victimization mobile part consisting of a combination of fifty volumes of Triethylamine buffer, fifty volumes of acetonitrile with detection of 230nm. Dimensionality was discovered within the vary 5-15 µg/ml for aceclofenac (r2 =0.999) and 1-3 µg /ml for tizanidine (r2 =0.998) for the number of medicine calculable by the planned strategies was in smart agreement with the label claim. The planned strategies have a sound procedure. At three completely different levels the accuracy of the strategies was assessed by recovery studies. The recovery experiments indicated the absence of interference from unremarkably encountered pharmaceutical additives showing %RSD below a pair of this technique was found to be precise as indicated by the repeatability analysis. All applied mathematics information proves all ways have valid procedure and might be used for routine analysis of pharmaceutical dose kind

Determination of the depth distribution of complex nanostructures by X-ray photoelectron spectroscopy (XPS) inelastic background analysis may be complicated if the sample materials have widely different inelastic scattering cross-sections. It was recently demonstrated that this may be solved by using a mixture of cross-sections. This permits retrieval of depth distributions of complex stacks and deeply buried layers with a typical 5% accuracy. This requires however that the cross-sections of the individual sample materials are known which is often not the case and this can complicate practical use for routine analysis. In this paper, we explore to what extent a suitable two- or three-parameter cross-section can be defined independent of prior knowledge of the cross-sections involved but simply defined by fitting the cross-section parameters to the spectrum being analyzed. This paper presents a theoretical study following our recent paper that explored how to make the best choice of inelastic mean free path and inelastic scattering cross-section for the inelastic background analysis with the Quases-Tougaard software. It was previously shown that a rough analysis of the inelastic background could give a good idea of the depth distribution. Here, we demonstrate with model spectra from buried layers created with Quases-Tougaard Generate software that a rather accurate analysis can be performed for very different cases with an average ~5% error. This analysis is easy to apply as it only needs the two- or three-parameter cross-sections generated with the Quases-Tougaard software. This study is aimed to improve routine analysis of the inelastic background of XPS and hard X-ray photoelectron spectroscopy (HAXPES) spectra.

Objectives: In the proposed study, a basic, novel, protected economic, delicate and cost-effective UV-Spectrophotometric technique for the analysis of Decitabine which is antineoplastic drug. Methods: The created method was approved according to ICH rules. The decitabine indicated maximum absorption at 221 nm. This strategy can successfully apply for estimation of Decitabine in active pharmaceutical ingredient (API) form for routine examination with UV identification at 221 nm. A Shimadzu UV-Visible spectrophotometer 1800 with 1 cm quartz cells and Acetonitrile (ACN) as diluent was utilized in this technique. Results: The Developed technique obeyed Beer's-Lambert's law in the conc. of 5.0-15.0 ug/ml, having R2 of 0.9993 and 99.82%±0.75 recovery of decitabine was found. Different approval parameters like linearity, accuracy, precision and robustness were performed and were found to be within the limits as per the guidelines of ICH

A simple way of computer implementation of an effective two-parameter subgrade model for the routine analysis of flexible foundations on an elastic subgrade is presented. It is based on a rigorous ...

A simple, accurate and precise colorimetric method was developed for the quantification of pregabalin (PGN) in bulk and pharmaceutical formulations. The method was based on the production of a colored complex by reacting PGN with ascorbic acid in DMSO solvent. The resultant complex exhibits absorption maxima at 390 and 532 nm. The factors that affect the complex development and stability were studied and optimized. The reaction stoichiometry of drug: reagent was found to be 1:2. The method was then validated according to ICH guidelines. Regression analysis of Beer's plot showed good correlation (r2 value more than 0.998) within a concentration range of 5-30μg/ml. Linearity was confirmed by standardized residuals versus fitted value plots using Minitab14 software. The limits of detection and quantification at 390 and 532nm were 1.34μg/ml, 1.09μg/ml and 4.05μg/ml, 3.294μg/ml, respectively. Added recovery measurements were found to be 100.04±2.07% and 99.58 ±1.98% at 390nm and 532nm, respectively, which reflect the accuracy of the method and freedom from interference (relative standard deviation values were less than or equal 0.2%). The average assay for the commercial capsule preparation (PGN 150mg/capsule) was found to be 101.373±0.49 and 101.812±0.73 at 390 and 532nm, respectively. The developed method is an inexpensive, extraction free and can be applied for routine analysis of PGN in most of analytical laboratories.

Baclofen (BLF) has been prescribed in the UK since 1972 for the alleviation of spasticity. However, evidence suggests BLF is also recreationally misused. It has been associated with ethanol, gamma-hydroxybutyric acid (GHB), pregabalin (PGL) and gabapentin (GBP) use/abuse, and deaths have been reported. With current postmortem (PM) toxicological screening approaches, BLF is not routinely included in the general drugs screen and is only screened for if specifically mentioned in the case documents. The extent of BLF misuse is thus unclear. This study was carried out to determine the prevalence and concentrations of BLF in Coroners’ toxicology, to investigate whether BLF misuse with ethanol, GHB, PGL and GBP is causing death and to determine the potential extent of the underreporting of BLF-associated deaths. Between 1 January 2016 and 31 December 2017, 3,750 PM femoral vein bloods were screened for BLF; all positive cases were quantified. Only 0.56% of samples screened positive for BLF, with concentration ranging from 0.08 to 102.00 µg/mL (median = 0.28). It was determined that if routine analysis without additional screening of BLF had been performed, 43% of BLF positives cases would have been missed. However, given the low incidence of detection, this only represents 0.25% of the cohort. Likely illicit use of BLF with GHB was seen in one case only. Death from the recreational use of BLF with PGL and GBP was not observed. Only two cases positive for BLF had an ethanol concentration of ≥50 mg%. Two cases of presumed intentional overdose of BLF were observed. This study highlights that although BLF abuse may be occurring, deaths are rare. It is therefore not cost- or time-effective to screen for BLF in all PM cases. With BLF currently being investigated for the treatment of alcoholism and withdrawal symptoms of illicit drug use, BLF-related deaths may rise in the future.

Vegan food claims to be free of all animal material. This must be verified by the food control authority and the production control laboratory. The method must be sensitive and able to detect animal material after processing such as pasteurization and storage. We have, therefore, developed a multiplex qPCR to simultaneously detect animal, fish and plant DNA in food samples. The system is cost-efficient and exhibited a high sensitivity. The specificity tests confirmed that all relevant species are detected. The plant-specific system served as a DNA isolation control and was used to generate valid results. A large selection of market samples had been analyzed and showed the expected results and the robustness of this analytical tool in routine analysis.

Objective: A new sensitive, economical, simple, rapid UV spectrophotometric method has been developed for the estimation of Saxagliptin in API and pharmaceutical formulation. Methods: Calibration curve method was used for the estimation of Saxagliptin in API and pharmaceutical formulation. Results: The method was validated for linearity, range, accuracy, precision, robustness, LOD, LOQ. Linearity was found in the range of 10-60µg/ml. Accuracy was performed by using a recovery study. The amount of drug recovered was found to be in the range of 99.01-100.1%. All the parameters were validated as per the ICH guidelines. Conclusion: This method is suitable forused routine analysis of present Saxagliptin in API and Pharmaceutical dosage form.

Food safety and quality issues are becoming increasingly important and attract much attention, requiring the development of better analytical platforms. For example, high-resolution (especially Orbitrap) mass spectrometry simultaneously offers versatile functions such as targeted/non-targeted screening while providing qualitative and quantitative information on an almost unlimited number of analytes to facilitate routine analysis and even allows for official surveillance in the food field. This review covers the current state of Orbitrap mass spectrometry (OMS) usage in food analysis based on research reported in 2012-2019, particularly highlighting the technical aspects of OMS application and the achievement of OMS-based screening and quantitative analysis in the food field. The gained insights enhance our understanding of state-of-the-art high-resolution mass spectrometry and highlight the challenges and directions of future research.

Разработана фотохимическая методика определения водорастворимых антиоксидантов, основанная на титровании аналита фотогенерированным йодом, полученным в результате облучения вспомогательного раствора, содержащего йодид калия, сенсебилизатор при рН 5,6. Так как содержание титранта в растворе контролировали вольтамперометрическим методом, стабилизация тока в ячейке свидетельствовала о полноте протекания реакции. Данная методика удовлетворяет параметрам валидации по показателям: линейность, прецизионность, правильность. Ее применение в аналитической практике позволяет снизить не только время единичного определения за счет отсуствия необходимости проведения стандартизации растворов и выполнения рутинного анализа, но и стоимость единичного анализа, так как не требует применения дорогостоящего оборудования и реактивов.

A simple, economical, rapid, accurate, precise spectrophotometric method has been developed and validated according to ICH Guidlines for the Mirabegron as active pharmaceutical ingredient (API) by UV spectrophotometric method. The absorption maxima of Mirabegron was found to be at 249 nm wavelength using 1N Hcl as a solvent. Linearity range was found to be 3-15μg/ml, with the correlation coefficient being more than 0.999. The relative standard deviation was found to be < 2%. The percentage recovery was within the range of 98% -105%, indicating that there is no significant interference from the other ingredients present in the formulation. The method can be applied for the routine analysis of Mirabegron as API in pharmaceutical preparation.

A rapid and accurate Reversed Phase-UHPLC method was developed for determination of gallic acid, quercetin and kaempferol in herbal drugs found in herbal product purchased from local market. A reversed phase chromatographic analysis was carried out under isocratic conditions using column Phenomenex, Prodigy, ODS3, 5.0 μm, 100 A, 250 × 4.6 mm (USA). The mobile phase was methanol and 0.5% phosphoric acid (50:50 v/v). The flow rate was 1.3 mL/min. The injection volume was 20 µL. The detection wavelength (λ max) was 370 nm using a PDA (photodiode array detector). Linearity of the method was established over the concentration ranges of 240 – 960 µg mL-1 for quercetin with a retention time about 7.8 minutes. Correlation coefficients was greater than 0.99. The recovery level of quercetin was 99.94%. The described method was quite suitable for routine analysis of herbal drugs by Reversed Phase-UHPLC Method.The proposed method was used for routine analysis to estimate the selected polyphenols under study in its pure form as well as in some herbal drugs forms.

A biomarker of doping indicates the biological response to the use of a prohibited substance or method. Uncovering novel biomarkers of doping is a key objective in order to improve antidoping outcomes such as the detection of doping and changing athlete behavior toward doping practices. While the antidoping field has been successful in validating novel metabolites of prohibited substances, there has been less success in developing new biomarkers of doping. Employing the most suitable study designs and analytical approaches is critical to successfully uncovering novel biomarkers of doping with a high potential for translation into routine analysis. Here we argue that the antidoping field is well positioned for biomarker discovery and outline considerations for the development of novel biomarkers of doping.

Sample pretreatment is the first and the most important step of an analytical procedure. In routine analysis, liquid–liquid microextraction (LLE) is the most widely used sample pre-treatment technique, whose goal is to isolate the target analytes, provide enrichment, with cleanup to lower the chemical noise, and enhance the signal. The use of extensive volumes of hazardous organic solvents and production of large amounts of waste make LLE procedures unsuitable for modern, highly automated laboratories, expensive, and environmentally unfriendly. In the past two decades, liquid-phase microextraction (LPME) was introduced to overcome these drawbacks. Thanks to the need of only a few microliters of extraction solvent, LPME techniques have been widely adopted by the scientific community. The aim of this review is to report on the state-of-the-art LPME techniques used in gas and liquid chromatography. Attention was paid to the classification of the LPME operating modes, to the historical contextualization of LPME applications, and to the advantages of microextraction in methods respecting the value of green analytical chemistry. Technical aspects such as description of methodology selected in method development for routine use, specific variants of LPME developed for complex matrices, derivatization, and enrichment techniques are also discussed.