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Tripropyl phosphate (TnPP) is a commonly used organic phosphate flame retardant in the textiles, plastics, and coating industries. Residues are commonly detected in samples from the environment and food. The availability of certified reference materials (CRMs) is essential to ensure the accuracy and traceability of detection results. In this study, a comprehensive characterization of a CRM for TnPP was carried out, and its purity was evaluated using two distinct methodologies: mass balance (MB) and quantitative nuclear magnetic resonance spectroscopy (qNMR). In the MB method, the levels of structurally related organic impurities are 1.37 mg/g. The water content was determined to be 3.16 mg/g, while inorganic impurities were found to be 0.87 mg/g, and no residual organic solvents were detected. Benzoic acid and monocrotophos were chosen as internal standards for 1H-qNMR and 31P-qNMR, respectively. The purity of the TnPP CRM was assessed as 994.6 mg/g, 994.1 mg/g, and 993.5 mg/g using MB, 1H-qNMR, and 31P-qNMR techniques, respectively. The verified purity of the TnPP CRM was ultimately determined to be 994.1 mg/g, with an expanded uncertainty of 3.4 mg/g (k = 2), ensuring traceability to the International System of Units (SI). This CRM can be effectively utilized for preparing calibration solutions suitable for the routine monitoring of TnPP residues in plastics and food samples. [ABSTRACT FROM AUTHOR]

Preparation of a novel TpBD (synthesized from phloroglucinol and benzidine) covalent organic framework (COF) immobilized open-tubular (OT) capillary is described by in situ growth strategy. The stationary phase in the column was characterized by Fourier transform infrared (FTIR) spectra, X-ray diffraction (XRD), thermogravimetric analysis (TGA), nitrogen adsorption–desorption isotherms, scanning electron microscope (SEM), transmission electron microscopy (TEM) and energy-dispersive X-ray spectrum (EDS). Several families of compounds with different properties (alkylbenzenes, parabens, sulfonamides and benzoic acids) were selected to evaluate the performance of the TpBD COF immobilized capillary. The results showed that the stationary phase was uniform with about 6.0 μm thickness under the optimal preparation conditions, and the relative standard deviations (RSDs) were no more than 3.13% of alkylbenzenes on the TpBD COF immobilized capillary for 11 consecutive runs, which exhibited its excellent reproducibility and stability. A rapid baseline separation of each family of the analytes (neutral parabens, amphoteric sulfonamides and acidic benzoic acids) was obtained in less than 6 min with a resolution (Rs) of 2.79~9.30, which sufficiently verified the rapid separation, high resolution and wide application range of the TpBD COF immobilized capillary, and further revealed this strategy of fabricating COF to capillary column to show great promise in capillary electrochromatography. [ABSTRACT FROM AUTHOR]

Simultaneous enantioseparation and rapid determination method of atenolol (AN) and amlodipine besylate (AMB) was firstly established using diphenylmethane diisocyanate-β-CD-modified COF (MDI-β-CD-modified COF) as chiral solid phases (CSP) by capillary electrochromatography (CEC). The optimal separation conditions were explored and the concentration of the acetate buffer solution was 20 mmol/L, pH = 5.0, operating voltage 20 kV, column temperature 20 °C, and then the four enantiomers of AN and AMB were baseline separated less than 5 min. The method validation was assessed by applying standard addition technique. The results showed that the concentration of each enantiomer exhibited a good linear relationship with the chromatographic peak area (r2 > 0.9918); the limit of detection (LOD) was 0.55–0.98 mg/L; the limit of quantification (LQD) was 1.83–3.27 mg/L; the average recoveries were in the range of 95.4–103.0%; the relative standard deviation (RSD) was less than 3.8%. The method established is rapid, simple, sensitive, accurate and reliable, and it can be used for routine analysis and quality control of the two chiral drugs separately or in combinations. [ABSTRACT FROM AUTHOR]

Covalent organic frameworks (COFs) have been recognized as promising solid phases in capillary electrochromatography (CEC). Imine‐based COF‐coated open‐tubular CEC column (COF TpBD‐coated OT column) was prepared and characterized by X‐ray diffraction (XRD), Fourier‐transform infrared (FT‐IR) spectra, thermogravimetric analysis (TGA), nitrogen adsorption/desorption (Brunauer–Emmett–Teller [BET]), and scanning electron microscopy (SEM). The results showed that the column efficiency was up to 26,776 plate/m, and the thickness of stationary phase was about 6.00 μm for the column prepared under the optimal conditions. Enantioseparation of 15 kinds of the single chiral compounds (histidine, arginine, lysine, leucine, threonine, methionine, valine, aspartic acid and glutamic acid, fipronil, diclofop, imazamox, quizalofop‐p, imazethapyr, and acephate) and 3 kinds of mixed amino acids racemaces (valine, methionine, and glutamic acid) were performed with three methods: capillary electrochromatography with COF TpBD‐coated OT column (Method 1), CEC with COF TpBD‐coated OT column as the separation channels, and capillary electrophoresis (CE) with HP‐β‐CD as the chiral mobile phase additive (Method 2) and CE with HP‐β‐CD as the chiral mobile phase additive (Method 3). Separation efficiency and chiral selectivity of Method 2 was best among the three methods. Under the optimal separation conditions of Method 2, all the enantiomers reached the baseline separation regardless of the single chiral compounds or the mixed amino acids. Relative standard deviation (RSDs) of the mean column efficiency for reproducibility and stability was in the range of 0.46–1.49%. This combination of CEC and CE has great potential for use in chiral separation. [ABSTRACT FROM AUTHOR]

Luminescent Ln-MOFs (Eu0.075Tb0.925-MOF) were successfully synthesised through the solvothermal reaction of Tb(NO3)3·6H2O, Eu(NO3)3·6H2O, and the ligand pyromellitic acid. The product was characterised by X-ray diffraction (XRD), TG analysis, EM, X-ray photoelectron spectroscopy (XPS), and luminescence properties, and results show that the synthesised material Eu0.075Tb0.925-MOF has a selective ratio-based fluorescence response to Fe3+ or Cr2O72−. On the basis of the internal filtering effect, the fluorescence detection experiment shows that as the concentration of Fe3+ or Cr2O72− increases, the intensity of the characteristic emission peak at 544 nm of Tb3+ decreases, and the intensity of the characteristic emission peak at 653 nm of Eu3+ increases in Eu0.075Tb0.925-MOF. The fluorescence intensity ratio (I653/I544) has a good linear relationship with the target concentration. The detection linear range for Fe3+ or Cr2O72− is 10–100 μM/L, and the detection limits are 2.71 × 10−7 and 8.72 × 10−7 M, respectively. Compared with the sensor material with a single fluorescence emission, the synthesised material has a higher anti-interference ability. The synthesised Eu0.075Tb0.925-MOF can be used as a highly selective and recyclable sensing material for Fe3+ or Cr2O72−. This material should be an excellent candidate for multifunctional sensors. [ABSTRACT FROM AUTHOR]