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A sensitive, stability-indicating reversed-phase high-performance liquid chromatography with diode array detection (HPLC–DAD) method has been developed for the determination of TBI-166 and its 10 kinds of related impurities. Chromatographic separation was achieved on a Kromasil ODS column (250 mm × 4.6 mm, 5 μm), with a gradient elution of the mobile phase system consisting of acetonitrile and 1% ammonium formate solution (with 0.2% formic acid). The flow rate was 1.0 mL/min, and the detection wavelength was set at 251 nm. The method was validated according to the International Conference on Harmonization (ICH) guidelines with respect to selectivity, linearity, limits, accuracy, precision, and robustness. The calibration curves were linear from LOQ to 150% of the specification limit of impurity with correlation coefficients not less than 0.999. The limits of quantitation were between 0.123 and 0.257 μg/mL. Accuracy for the related substances was estimated by the recovery ranged from 94.6% to 111.2%. The method was proved to be reliable for the determination of related substances in TBI-166 bulk drug, which is essential and important in the quality control.

Open access
Acta Chromatographica
Authors: Yun Wang, Jianhong Chen, Yutian Li, Puling Li, Javed Iqbal, Ying Chen, Yinlian Ma, and Cun Zhang

A reliable and rapid high-performance liquid chromatography coupled with diode array detector method (HPLC–DAD) was established and validated to determine eight gingerol simultaneously in the rhizomes of Zingiber offcinale Rosc. The separation of eight compounds (4-hydroxy-3-methoxy-benzenebutanol,3,5-dihydroxy-1-(4-hydroxy-3-methoxyphenyl) decane, 3,5-dihydroxy-1-(3,4-dimethoxyphenyl) decane, 6-gingerol, 8-gingerol, 6-shogaol, 5-hydroxy-1-(4-hydroxy-3-methoxyphenyl)-1,4-decadien-3-one, and 10-gingerol) were performed on an Agilent TC(2) C18 (250 mm × 4.6 mm, 5 μm) at 30 °C using acetonitrile (A) and 1% formic acid aqueous solution (B) as the mobile phase with gradient elution (0–10 min, 20%–35% A; 10–28 min, 35%–55% A; 28–35 min, 55%–60% A; 35–55 min, 60%–70% A; 55.01–60 min, 100%–100% A). The detection wavelength was set at 280 nm, and the flow rate was 0.8 mL/min. Validation of the analytical method was performed by linearity, precision, and accuracy test. All compounds were quantified with good linear calibration curves (coefficient of determination R 2, >0.9999). The method showed good precision with overall coefficients of variation between 0.56% and 0.84%. The range of recovery was from 95.50% to 104.14% for the analytes. This method was successfully applied to quantify eight gingerols in Z. offcinale Rosc from different regions in China, so it can provide quality assessment for this medicine.

Open access

A modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method and ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry (UHPLC–MS/MS) were optimized and validated for 16 antibiotics belonging to three families (macrolides, quinolones, and sulfonamides) that were found in preserved eggs. Samples were extracted in 4 mL water and 10 mL acetonitrile with 1% acetic acid and subjected to a cleanup procedure using dispersive solid-phase extraction with C18 and primary secondary amine sorbents, prior to detection by UHPLC–MS/MS. Matrix-matched calibration was used for quantification to reduce the matrix effect with limits of quantification in the range of 0.3–3.0 μg/kg. Validation of the method was conducted by recovery and precision experiments. Recoveries of the spiked samples ranged from 73.8% to 127.4%, and the intra- and inter-day relative standard deviations were lower than 21.2% and 22.3%, respectively. This method was successfully applied to the analysis of antibiotics in preserved egg samples.

Open access

RKI-1447 is an effective ROCK1 and ROCK2 inhibitor, having anti-invasion and anti-tumor activity. In this study, we used ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) to detect RKI-1447 in rat plasma and investigated its pharmacokinetics in rats. Diazepam was utilized as an internal standard, and an acetonitrile precipitation method was used to process the plasma samples. Chromatographic separation was achieved using a UPLC ethylene bridged hybrid (BEH) column (2.1 mm × 50 mm, 1.7 μm) with a gradient acetonitrile–water mobile phase (containing 0.1% formic acid). Flow rate was set at 0.4 mL/min. Electrospray ionization (ESI)–tandem mass spectrometry in multiple reaction monitoring (MRM) mode with positive ionization was applied: m/z 327.1 → 204.0 and 285.1 → 193.3 for RKI-1447 and internal standard, respectively. The results indicated that within the range of 10–2000 ng/mL, the linearity of RKI-1447 in rat plasma was acceptable (r > 0.995), and the lowest limit of quantification (LLOQ) was 10 ng/mL. Intra-day precision RSD of RKI-1447 in rat plasma was lower than 8%, and inter-day precision RSD was lower than 11%. Accuracy range was between 91.6% and 107.1%, and the matrix effect was between 85.1% and 87.0%. The analysis method was sensitive and fast with suitable selectivity, and was successfully applied in the pharmacokinetics of RKI-1447 in rats. The bioavailability of the RKI-1447 was 7.3%.

Open access

Abstract

The aim of the experiment is to establish a method for the determination of acrylamide in food by automatic accelerated solvent extraction-gas chromatography-mass spectrometry. D3-acrylamide was used as isotope internal standard, crushed samples were extracted and purified by automatic accelerated solvent, acrylamide was derivatized into 2,3-dibromopropanamide by potassium bromide and potassium bromate under acidic conditions, and then the derivative was extracted by ethyl acetate and detected by gas chromatography-mass spectrometry. The method had a good linear relationship in the concentration range of 10–2000 ng/mL, and the coefficient of determination (R2) was 0.9997. The detection limit of the method was 3 μg/kg. The quantification limit of the method was 10 μg/kg. The standard addition recovery of acrylamide was between 105 and 120%, and the relative standard deviation of the recovery of acrylamide was less than 3.0%. The experimental result showed that the method was simple, sensitive, efficient and accurate, and could be used for the determination of acrylamide in food.

Open access

Summary

A reversed-phase chiral liquid chromatographic method had been developed and validated for resolution of the enantiomers of racemic fudosteine. The effects on the separation of the amounts of anhydrous cupric sulfate and l-phenylalanine, the methanol content, mobile phase pH, and temperature were investigated. The method was validated for linearity, repeatability, intermediate precision, sample recovery, solution stability, and limits of detection (LOD). l-Phenylalanine and anhydrous cupric sulfate as chiral ligand-exchange complexes were used for separation, isomer identification, related substance investigation, and analysis of fudosteine enantiomers in fudosteine bulk drugs and fudosteine tablets.

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