毛细管气相色谱法测定头发中尼古丁及其代谢产物可的宁

目的建立毛细管气相色谱同时测定头发中尼古丁及其主要代谢产物可的宁的方法。方法头发样品经1.5mol/L NaOH溶液消解,二氯甲烷/甲醇(V/V,3∶1)溶剂萃取,氮气吹干,甲醇定容后直接进样。经SPB-5毛细管柱分离,火焰离子化检测器(FID)检测。结果在优化发样提取和色谱分析条件下,尼古丁和可的宁在4.3ng/mL~1mg/mL和10ng/mL~2mg/mL浓度范围内线性良好(r均为0.9996),方法检出限(S/N=3)分别为4.3ng/mL和10ng/mL。发样中尼古丁和可的宁的加标回收率分别为90.33%~113.1%和92.92%~117.4%,相对标准偏差为2.1%~7.0%和4.4%~8.9%。结论本方法灵敏度高,选择性好,操作简便、快速,易于推广,可用于控烟流行病调查研究批样的检测。

Detecting Nicotine and Its Metabolite Cotinine in Human Hair with Capillary Gas Chromatography

OBJECTIVE: To develop a rapid method for determination of nicotine and its metabolite cotinine in human hair with capillary gas chromatography with flame ionization detector. METHODS: The hair sample was digested by 1.5 mol/L sodium hydroxide solution. The nicotine and cotinine in the hair sample were extracted with a mixed solvent of dichloromethane-methanol (3:1). Aliquot of the extraction solution was vaporized with nitrogen flow and then methanol was added to dissolve the analysts. The analysts were tested with capillary gas chromatography. RESULTS: The detection limits (signal to noise ratio of 3:1) were 4.3 ng/mL for nicotine and 10 ng/mL for cotinine, respectively. The spiked recoveries were 90.33%-113.1% for nicotine with relative standard deviation (RSD) of 2.1%-7.0% and 92.92%-117.4% for cotinine with relative standard deviation (RSD) of 4.4%-8.9%, respectively. CONCLUSION: The proposed method is sensitive, simple, easy and rapid. It can be easily extended to large scale applications in tobacco epidemiology studies.