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Validation and quantification of a UPLC-MS/MS method for the simultaneous determination of quinocetone and its main metabolites (3-methylquinoxaline-2-carboxylic acid and dedioxoquinenone) in aquatic products

Tian Xiuhui, Han Dianfeng, Cui Yanmei, Ren Lihua, Jiang Fang, Huang Hui, Gong Xianghong, Xue Jinglin, Li Jiawei, Liu Huihui, Xu Yingjiang, Luo Xiaojun, Liu Xiaojing, Zhang Xiuzhen

Acta Chromatographica

2022

Vol. 34, no. 4

444--452

A sensitive and validated method for determining quinocetone and its main metabolites (3-methylquinoxaline-2-carboxylic acid and dedioxoquinenone) was established in aquatic products using ultra-high-performance liquid chromatography-tandem spectrometry (UHPLC-MS/MS). Samples were extracted with 2.0 mol L⁻¹ hydrochloric acid, then purified on MAX columns. After extraction and purification, the supernatant was evaporated to dry nearly under a gentle stream of nitrogen at 40 °C. Formic acid-acetonitrile-water (0.1/30/70, v/v/v) was adjusted to 1.00 mL final volume. An aliquot (10 μL) was injected into the C18 column for separation with the mobile phase of acetonitrile and 0.5% formic acid in water at 0.25 mL min⁻¹. Calibration curves were linear ranged from 10.00 ng mL⁻¹ to 200.0 ng mL⁻¹ for quinocetone and 3-methylquinoxaline-2-carboxylic acid, and 20.00 ng mL⁻¹ to 400.0 ng mL⁻¹ for dedioxoquinenone. Mean recoveries were 70%–89%, 73%–83% and 72%–84%, respectively. The limit of detection (LOD) was 1.00 μg kg⁻¹, 1.00 μg kg⁻¹ and 2.00 μg kg⁻¹, and quantification (LOQ) were 2.00 μg kg⁻¹, 2.00 μg kg⁻¹ and 4.00 μg kg⁻¹ for quinocetone, 3-methylquinoxaline-2-carboxylic acid, and dedioxoquinenone. Based on the method above, the analytes were determined in Apostichopus japonicus, three fishes (including Ctenopharyngodon idellus, Crucian carp and Oreochromis mossambicus), Penaeus vannamei, Penaeus chinensis, and Chlamys farreri. The method shows good sensitivity, linearity, precision, and accuracy. In short, the proposed method was reliable for the determination of quinocetone, 3-methylquinoxaline-2-carboxylic acid, and dedioxoquinenone in aquatic products.

Simultaneous determination of carbofuran and 3-hydroxycarbofuran in duck liver by an UPLCMS/MS

Chen Siyuan, Yu Yang, Ma Jianshe, Wen Congcong, Wang Xianqin, Zhou Quan

Acta Chromatographica

2021

Vol. 33, no. 4

354--360

Carbofuran is a carbamate pesticide, a broad-spectrum, high-efficiency, low-residue, and highly toxic insecticide, acaricide, and nematicide, widely used in agriculture. Carbofuran is most harmful to birds, and birds or insects killed by furan poisoning can be killed by secondary poisoning after being foraged by raptors, small mammals, or reptiles. In this paper, an UPLC-MS/MS method was developed for the determination of carbofuran and its metabolite, 3-hydroxycarbofuran, in duck liver. Liver tissue was first ground into a homogenate and then passed through ethyl acetate liquid-liquid extraction processing samples. Multiple reaction monitoring (MRM) mode was used for quantitative analysis, m/z 222.1 → 165.1 for carbofuran, m/z 238.1 → 180.9 for 3-hydroxycarbofuran and m/z 290.2 → 198.2 for an internal standard. The standard curves of carbofuran and 3-hydroxycarbofuran in duck liver were within a range of 2–2000 ng/g, where the linearity was good, the lower limit of quantification was 2 ng/ g. The intra-day precision of carbofuran and 3-hydroxycarbofuran was <14%, and the inter-day precision was <13%, the accuracy range was between 91.8 and 108.9%, the average extraction efficiency was higher than 75.1% with a matrix effect between 93.4 and 107.7%. The developed method was applied to a situation of suspected duck poisoning at a local farm.

A rapid and sensitive UPLC–MS/MS method for determination of remimazolam and its main metabolite in human urine and its application in clinical urine recovery study

Zhou Y., Lu M., Jiang J.

Acta Chromatographica

2018

Vol. 30, no. 2

109--113

Remimazolam is a new chemical entity belonging to the benzodiazepine class of sedative drugs. A sensitive and rapid method based on ultra-performance liquid chromatography–tandem mass spectrometry (UPLC–MS/MS) has been developed and validated for the determination of remimazolam and its major carboxylic acid metabolite (M1) in human urine. Urine samples were prepared by dilution and analyzed using an isocratic chromatographic separation. Inter- and intra-batch results for remimazolam were within 10.7% for accuracy and 5.5% for precision, and for M1, within 5.8% for accuracy and 4.2% for precision, respectively. This study represents the first reported example for the quantification of remimazolam and its main metabolite in human urine. Furthermore, this method has been successfully applied for the urine recovery study of remimazolam in Chinese healthy subjects. Only about 0.01% of the administered remimazolam dose was eliminated in the urine over the 24 h period in the form of unchanged remimazolam, and more than 75.1% of the administered dose was eliminated in the form of M1. Remimazolam is excreted mainly in the form of M1 in urine after intravenous administration, and there is no excessive accumulation in vivo after administration of remimazolam.