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Abstract

High-performance liquid chromatography with a hydrophilic-interaction liquid chromatographic (HILIC) column has been successfully used to retain and separate the polar phosphonic herbicides glyphosate and glufosinate. Online electrospray tandem ion-trap mass spectrometric and DAD detection were used. The effects on the separation of mobile phase acetonitrile content, buffer concentration, and flow rate, and of column temperature, were investigated. With UV-visible detection at 195 nm, LOQ were <850 mg kg−1, showing the method is suitable for product quality control of these herbicides alone or in combination. Tandem mass spectrometric conditions were optimized for ion-trap detection. Quantification was by use of selected reaction monitoring transitions m/z 168 → 150 in negative-ion mode for glyphosate and m/z 182 → 136 in positive-ion mode for glufosinate. Limits of detection (LOD; S/N > 3) were 0.20 and 0.16 ng for glyphosate and glufosinate, respectively, and the respective limits of quantification (LOQ; S/N = 10) were 0.02 and 0.05 mg kg−1. Sample derivatization was not necessary to achieve low detection limits in residue analysis in this study. Recovery from watermelon, spinach, potato, tomato, radish-root, and water fortified with the herbicides ranged from 63.6 to 107.3% and relative standard deviations were <15.3%.

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Cortisol and cortisone are 2 important glucocorticoids produced in the human hypothalamus–pituitary–adrenal (HPA) axis that respond to stress. An analytical method to determinate cortisol and cortisone in serum and saliva using high-performance liquid chromatography–tandem mass spectrometry following a supported liquid extraction (SLE) was developed. Serum and saliva samples of 0.2 mL were extracted by SLE three times using 0.4 mL of methyl tert-butyl ether each time. The chromatographic separation was obtained on an Agilent Poroshell column using a 0.01% formic acid buffer and acetonitrile (60:40, v/v) as the solvent with a flow rate of 0.3 mL/min. Optimized quantitative mass transitions for cortisol, cortisone, and cortisone d-4 were 363.2/121.0 (m/z), 361.2/163.1 (m/z), and 367.1/270.7 (m/z), respectively. The method validation was achieved according to regulatory guidance. The lower limit of quantification (LLOQ) in serum were 2 ng/mL for cortisol and 1 ng/mL for cortisone, and the LLOQ in saliva were 0.1 ng/mL for cortisol and 0.2 ng/mL for cortisone. The developed method showed convenient and efficient extraction, a lower LLOQ, and a short running time. Modest correlations between serum and saliva cortisol and cortisone concentrations were found. The method was successfully applied in assessing the HPA condition of patients with depressive disorders.

Open access
Acta Chromatographica
Authors: Weijian Ye, Wei Sun, Ruijie Chen, Zhe Wang, Xiao Cui, Hui Zhang, Shuyi Qian, Qi Zheng, Yangfeng Zhou, Jiafeng Wan, Jiali Xu, Xianqin Wang, and Yunfang Zhou

Galangin (GAL), the major bioactive flavonol extracted from Alpinia officinarum Hance (Zingiberaceae), has attracted much attention due to its multiple biological activities. To develop a fast, reliable, and sensitive ultrahigh-performance liquid chromatography–tandem mass spectrometry (UHPLC–MS/MS) method for the quantification of GAL in rat plasma and mouse tissues. UHPLC–MS/MS using electrospray ionization operating in negative-ion mode was used to determinate GAL in 18 rats receiving three doses of GAL (2 and 9 mg/kg by intravenous injection, 5 mg/kg by oral administration), with six rats for each dose. Blood samples were collected at 0.0333, 0.25, 0.5, 1, 2, 4, 6 and 8 h. A total of 25 mice received 18 mg/kg GAL by intraperitoneal injection. Liver, heart, lung, spleen, brain, and kidney tissue samples were collected at 0.25, 0.5, 2, 4, and 6 h. The precision of the method was better than 12.1%, while the accuracy ranged from −4.8% to 8.1%. The results of pharmacokinetics demonstrated rapid GAL absorption (t max of 0.25 h), fast elimination (t 1/2 <1.1 h) after three different dosages, and an absolute bioavailability of ~7.6%. Tissue distribution analysis revealed abundant GAL in liver, kidney, spleen, and lung and smaller amounts in brain. The developed method proved fast (3 min), efficient, and reliable, with high selectivity for the quantitative analysis of GAL in biological samples. This is the first study to identify the target tissues of GAL, and the results may help to elucidate the mechanisms underlying its therapeutic effects in vivo.

Open access

Abstract

A rapid and sensitive High-Performance Liquid Chromatography-tandem Mass Spectrometry (HPLC/MS/MS) method for determining apremilast in beagle dog plasma and urine samples was developed and validated using clopidogrel as the internal standard (IS). Apremilast was extracted from the plasma and urine samples by liquid–liquid extraction using methyl tert-butyl ether. Chromatographic separation was performed using a C8 column with gradient elution and a mobile phase containing methanol and 0.1% formic acid. Quantification was achieved in multiple reaction monitoring (MRM) mode with a transition of m/z 461.3→178.2 for apremilast and m/z 322.2→184.1 for clopidogrel (IS). This method was validated regarding its specificity, linearity, precision, accuracy, and stability. The lower limit of quantification (LLOQ) for this method was 5 ng/mL, and the calibration curve was linear over 5–1,000 ng/mL. The intra- and inter-run coefficients of variance (CV) of aprelimast in plasma samples were less than 12.92% and 10.64%, respectively, while in urine samples, the CV were less than 11.84% and 10.20%, respectively. The samples were stable under the tested conditions. This method was successfully applied to a pharmacokinetic study in beagle dogs following oral administration of 10 mg of apremilast.

Open access