QuEChERS-气相色谱/质谱法同时测定尿液中7种芬太尼类物质

Simultaneous Determination of Seven Fentanyls in Urine by QuEChERS Coupled with Gas Chromatography/Mass Spectrometry

建立了QuEChERS法结合气相色谱/质谱联用技术同时测定尿液中7种芬太尼类物质。尿液样品用0.2 mol/L pH=8的磷酸盐缓冲溶液调节pH,添加NaCl盐析,无水Na_(2)SO_(4)除水后用乙酸乙酯提取,并通过C18净化乙酸乙酯中的杂质后,供气相色谱/质谱法(GC-MS)检测。结果表明,使用5 mL乙酸乙酯作为提取溶剂,4 g无水Na_(2)SO_(4)作为除水剂,10 mg C18作为净化剂时,萃取效果最佳。在此条件下,7种芬太尼类物质在20.0~200.0 ng/mL范围内线性良好(R^(2)≥0.9988),检出限为0.44~3.33 ng/mL,定量限为1.47~11.11 ng/mL。当标准添加水平为20、100、200 ng/mL时,回收率范围为96.24%~118.27%。本方法操作简单、结果准确,可用于药物滥用人员尿液中芬太尼类物质的定性定量检测。

A method for simultaneous determination of seven fentanyls in urine by QuEChERS(Quick,Easy,Cheap,Effective,Rugged,Safe)combined with gas chromatography-mass spectrometry(GC-MS)was established.The urine samples collected from addicts was adjusted by 0.2 mol/L pH 8 phosphate buffer solution,salted out by sodium chloride,dehydrated by anhydrous sodium sulfate,and extracted with ethyl acetate.The impurities in the ethyl acetate were purified by octadecylsilane(C18)for GC-MS testing.The effects of extraction solvent,desiccant agent and amount of purifying agent were investigated.Under optimal conditions,the linear ranges of seven kinds of fentanyls were 20.0-200.0 ng/mL(R^(2)≥0.9988),the limits of detection(LOD)were 0.44-3.33 ng/mL,and the limits of quantification(LOQ)were 1.47-11.11 ng/mL.The recoveries were 96.24%-118.27%,at the spiked levels of 20,100 and 200 ng/mL.This method is simple and accurate,and can be used for urine testing of addicts.