气相色谱-氮磷检测方法同时检测尿样中的刺激剂、麻醉剂和抗雌激素类五种兴奋剂

建立了一种简单、灵敏、快速地同时测定人体尿液中3类(刺激剂、麻醉剂和抗雌激素)5种兴奋剂的气相色谱-氮磷检测(GC-NPD)方法。尿样采用非衍生法液-液萃取预处理技术,选用叔丁基甲醚作为萃取溶剂,二苯胺作为内标进行定量检测。即在一定量标准品及内标的混合溶液中加入5.0 mL空白尿样混合均匀后,加入0.5 mL 5 mol/L 氢氧化钠溶液、3.0 g 氯化钠和5.0 mL叔丁基甲醚提取液,涡旋、离心,萃取液经氮气吹干、丙酮溶解后用GC-NPD测定。该方法在0.022～20 mg/L之间呈现良好的线性关系,相关系数为0.9945～0.9998,最小检出质量浓度为0.007～0.015 mg/L。5种兴奋剂的尿样加标回收率为75.8%～118.2%,相对标准偏差小于17.2%。

Simultaneous determination of stimulant, narcotics and antiestrogen in urine by gas chromatography-nitrogen phosphorous detection

An easy, sensitive and quick method was established for simultaneously separating and determining stimulant, narcotics and antiestrogen in spiked human urine using gas chromatography-nitrogen phosphorous detection (GC-NPD). The urine sample was preprocessed by liquid-liquid extraction. Tert-butyl methyl ether and N-phenylamine were chosen as extraction solvent and internal standard for quantitation, respectively. That is, a standard stock mixture containing methylephedrine, meperidine, methadone, tamoxifen, fentanyl and N-phenylaniline was added into 5.0 mL urine samples and mixed uniformly, then 0.5 mL 5.0 mol/L NaOH, 3.0 g NaCl and 5.0 mL tert-butyl methyl ether were added and finally centrifuged. The extraction solution was dried under N2, redissolved by acetone and then determined by GC-NPD. The method showed the satisfactory linearity was between 0.022~20 mg/L, with the coefficient correlation from 0.9945 to 0.9998. The detection limits were in the range of 0.007~0.015 mg/L, and the average recoveries in spiked urine were between 75.8%~118.2% and the relative standard deviations were lower than 17.2%.