Citation: XU Fangmin, LI Haibo, WEI Wanli, LIU Lingyun, LI Qiang. Solvent with switchable hydrophilicity used in liquid-liquid microextraction combined with gas chromatography-mass spectrometry for the determination of diclazepam in urine[J]. Chinese Journal of Chromatography, ;2018, 36(10): 1067-1072. doi: 10.3724/SP.J.1123.2018.05022 shu

Solvent with switchable hydrophilicity used in liquid-liquid microextraction combined with gas chromatography-mass spectrometry for the determination of diclazepam in urine

XU Fangmin ^1, ,
LI Haibo ² ,
WEI Wanli ³ ,
LIU Lingyun ¹ ,
LI Qiang ²

1.
Institute of Forensic Science, Public Security Bureau of Jiangyin, Jiangyin 214431, China;
2.
Institute of Forensic Science, Public Security Bureau of Changzhou, Changzhou 213001, China;
3.
Institute of Forensic Science, Public Security Bureau of Wuxi, Wuxi 214001, China

Received Date: 4 June 2018

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. N,N-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% (n=6). The linear range was found to be 0.025-2.5 mg/L, with r² 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.
- liquid-liquid microextraction,
- gas chromatography-mass spectrometry,
- diclazepam,
- urine,
- switchable hydrophilicity solvent
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