Beijing Advanced Innovation Center for Food Nutrition and Human Health, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.
Shenzhen Center for Disease Control and Prevention, Shenzhen 518055, China.
Molecules. 2018 Dec 5;23(12):3215. doi: 10.3390/molecules23123215.
A rapid, reliable, and sensitive method was developed for the determination of ten tranquilizers in swine urine. Sample preparation was based on solid-phase extraction, which combined isolation of the compounds and sample cleanup in a single step. Separation was performed on a reversed phase C column by gradient elution with a chromatographic run time of seven minutes, consisting of 0.1% formic acid in water and acetonitrile as the mobile phase. Multiple reaction monitoring in positive mode was applied for data acquisition. Matrix-matched calibration was used for quantification and good linearity was obtained with coefficients of determination higher than 0.99. The average recoveries of fortified samples at concentrations between 0.05 and 10 µg/L ranged from 85% to 106% with interday relative standard deviations of less than 13% in all cases. The limits of detection and limits of quantification obtained for tranquilizers in the urine were in the ranges of 0.03⁻0.1 µg/L and 0.05⁻0.25 µg/L, respectively. The applicability of the proposed method was demonstrated by analyzing real samples; diazepam was detected at concentrations between 0.3 and 0.6 μg/L.
建立了一种快速、可靠、灵敏的检测猪尿液中十种镇静剂的方法。样品前处理基于固相萃取，在一步中完成化合物的分离和样品净化。采用反相 C 柱，以水和乙腈中的 0.1%甲酸作为流动相进行梯度洗脱，色谱运行时间为 7 分钟。采用正离子多反应监测模式进行数据采集。采用基质匹配校准进行定量，所有浓度在 0.05 至 10 µg/L 之间的加标样品的平均回收率在 85%至 106%之间，日内相对标准偏差均小于 13%。在尿液中检测到的镇静剂的检测限和定量限分别在 0.03⁻0.1 µg/L 和 0.05⁻0.25 µg/L 范围内。通过分析实际样品验证了该方法的适用性；在 0.3 至 0.6 µg/L 之间检测到了地西泮。
