固相萃取-气相色谱法测定人尿中尼古丁和可的宁  

DETERMINATION OF NICOTINE AND COTININE IN HUMAN URINE WITH SOLID-PHASE EXTRACTION AND GAS CHROMATOGRAPHY

作　　者：雍莉[1,2] 黎源倩[1] 肖全伟[1] 谷素英[1] 李磊[1] 马少俊 杨功焕 

机构地区：[1]四川大学华西公共卫生学院,成都610041 [2]四川省疾病预防控制中心 [3]中国防和医科大学流行病学教研室

出　　处：《现代预防医学》2009年第3期532-534,共3页Modern Preventive Medicine

摘　　要：[目的]建立固相萃取-气相色谱同时测定人尿样品中尼古丁及其代谢产物可的宁的方法。[方法]采用C18固相萃取小柱富集、净化尿液中的尼古丁和可的宁,尿液用磷酸盐缓冲液(pH=7.5)调节pH值后上柱,用0.4%氨水溶液(v/v)淋洗杂质,甲醇-4%醋酸(90:10,v/v)洗脱待测物,氮气吹干定容后,用气相色谱-火焰离子化检测器测定,根据保留时间定性,标准曲线法定量。[结果]尼古丁和可的宁的线性范围分别为0.10～100μg/ml和0.20～200μg/ml。对5ml尿样,该方法的最低检出浓度为尼古丁0.6ng/ml和可的宁1.2ng/ml。尼古丁和可的宁测定的相对标准偏差(RSD)分别为2.50%～4.70%和4.20%～5.10%,加标回收率分别为80.00%～88.00%和78.85%～103.8%。[结论]所建立的同时测定人尿中的尼古丁及其代谢产物可的宁的固相萃取-气相色谱法,具有快速、简便、分析成本低等优点,适用于大量样品的检测,可为人群吸烟行为的干预提供试验数据。[Objective] To develop a new method for determination of nicotine and its metabolite cotinine in human＇ s urine by solid-phase extraction （SPE） -gas chromatography with flame ionization （GC-FID）. [ Methods ] Nicotine and cotinine in urine were enriched and purified by solid-phase extraction using C18 cartridge. After being adjusted to pH7.5 with phos- phate buffer solution （PBS）, the urine sample was washed with 0.4% ammonia solution and eluted with methanol-acetic acid solution. The elution was evaporated with nitrogen and analyzed by GC-FID. The contents of nicotine and cotinine in samples were determined with calibration curve. [ Results] The linear ranges were 0.10μg/ml-100μg/ml. 0.20μg/ml-200 （g/ml and the detection limits of the method were 0.6ng/ml and 1.2ng/ml for nicotine and eotinine for 5.0ml of urine respectively. The precision of samples was 2.50%-4.70%, 4.20%-5.10% and the recoveries of the spiked samples ranged from 80.00%-88.00% and 78.85%-103.8% for nicotine and cotinine, respectively. [Conclusion3 The proposed method is proved to be sensitive, accurate, low expense. It is satisfying for determination of abundance samples. The study provides reliable experimental method and laboratory data for epidemiological investigation and smoke behavior intervention.

关 键 词：尿 尼古丁 可的宁 固相萃取法 气相色谱法 

分 类 号：R446.12[医药卫生—诊断学]