Xu Fangmin, Li Haibo, Wei Wanli, Liu Lingyun, Li Qiang
Institute of Forensic Science, Public Security Bureau of Jiangyin, Jiangyin 214431, China.
Institute of Forensic Science, Public Security Bureau of Changzhou, Changzhou 213001, China.
Se Pu. 2018 Oct 8;36(10):1067-1072. doi: 10.3724/SP.J.1123.2018.05022.
A simple, fast, and sensitive method was developed for the determination of diclazepam in urine using a solvent with switchable hydrophilicity in liquid-liquid microextraction followed by gas chromatography-mass spectrometry. -Dimethylcyclohexylamine was used as the extraction solvent with switchable hydrophilicity, because it can be made miscible or immiscible with aqueous phase by adding hydrochloric acid and sodium hydroxide. Experimental parameters affecting the extraction efficiency, such as the volume of hydrochloric acid, the type and volume of the solvent with switchable hydrophilicity, the volume of sodium hydroxide, and the extraction time, were investigated. Under the optimal conditions, the intraday and interday recoveries ranged from 76.5% to 90.3% with relative standard deviations between 3.3% and 6.5% (=6). The linear range was found to be 0.025-2.5 mg/L, with greater than 0.99 and limit of detection of 0.007 mg/L. This method provided excellent linearity, precision, and recovery, and thus, can be applied to the analysis of diclazepam in urine due to its simplicity, accuracy, and practicality.
开发了一种简单、快速且灵敏的方法，用于测定尿液中的地西泮。该方法采用具有可切换亲水性的溶剂进行液-液微萃取，随后进行气相色谱-质谱分析。使用二甲基环己胺作为具有可切换亲水性的萃取溶剂，因为通过添加盐酸和氢氧化钠，它可以与水相混溶或不混溶。研究了影响萃取效率的实验参数，如盐酸体积、具有可切换亲水性的溶剂类型和体积、氢氧化钠体积以及萃取时间。在最佳条件下，日内和日间回收率在76.5%至90.3%之间，相对标准偏差在3.3%至6.5%之间（n = 6）。线性范围为0.025 - 2.5 mg/L，相关系数大于0.99，检测限为0.007 mg/L。该方法具有出色的线性、精密度和回收率，因其简单、准确和实用性，可应用于尿液中地西泮的分析。
