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目的建立利用气相色谱-质谱(GC-MS)法同时测定人体尿液、头发、唾液中尼古丁及其代谢物可替宁的方法。方法将样品(消解完全的头发、尿液、唾液)经NaOH碱化后用三氯甲烷萃取,气相色谱分离,质谱检测采用选择离子扫描,并以二苯胺作为内标物进行定量。尿液中尼古丁和可替宁的浓度用尿肌酐校正。结果该方法的尼古丁和可替宁的检出限为分别为6.5、14.5 ng/ml,测定下限分别为22、48 ng/ml;尼古丁和可替宁的线性范围分别为0.022~4μg/ml、0.048~4μg/ml。尿液中尼古丁和可替宁的精密度分别为2.02%~2.62%、5.27%~7.24%;头发中尼古丁的精密度为1.09%~2.89%;唾液中可替宁的精密度为4.89%~4.54%。尿液中尼古丁及可替宁的加标回收率分别为82.76%~106.47%、81.87%~99.53%;头发中尼古丁的加标回收率为85.37%~103.91%;唾液中可替宁的加标回收率为80.92%~93.78%。结论该实验方法简单、快速、准确,能满足人群烟草暴露评价的需要。
Objective To establish a method for simultaneous determination of nicotine and its metabolite cotinine in human urine, hair and saliva by gas chromatography-mass spectrometry (GC-MS). Methods Samples (digested complete hair, urine, saliva) were alkalified by NaOH, extracted with chloroform, separated by gas chromatography, detected by mass spectrometry using selective ion scan, and quantified with diphenylamine as internal standard. Urinary nicotine and cotinine concentrations were corrected for urinary creatinine. Results The detection limits of nicotine and cotinine in this method were 6.5 and 14.5 ng / ml, respectively, with the lower limits of determination of 22 and 48 ng / ml, respectively. The linear ranges of nicotine and cotinine were 0.022-4 μg / ml, 0.048 ~ 4μg / ml. The precision of nicotine and cotinine in urine was 2.02% -2.62% and 5.27% -7.24% respectively. The nicotine in hair was 1.09% -2.89% and the cotinine in saliva was 4.89% 4.54%. The spiked recoveries of nicotine and cotinine in urine were 82.76% -106.47% and 81.87% -99.53%, respectively. The spiked recoveries of nicotine in hair were 85.37% -103.91% The recovery rate was 80.92% ~ 93.78%. Conclusion The experimental method is simple, rapid and accurate and can meet the needs of tobacco exposure assessment in the population.