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目的建立头发中尼古丁和可替宁的超高效液相色谱串联质谱(UPLC-MS-MS)测定方法。方法头发样品用Na OH溶液完全消解后用二氯甲烷+甲醇(3+1)萃取,以10 mmol/L乙酸铵(含0.1%甲酸)-乙腈作为流动相进行梯度洗脱,超高效液相色谱串联质谱多反应监测(MRM)模式测定,内标法定量。结果尼古丁在2~200μg/L的范围内,所得回归方程为y=1.296 7x-2.379 9,r=0.999 6;可替宁在0.2~20μg/L的范围内,所得回归方程为y=1.099 2x-0.005 15,r=0.999 9。以3倍信噪比计算,当取样量为50 mg时,尼古丁和可替宁检出限分别为0.01μg/g和0.001μg/g。该方法所得尼古丁的平均回收率在75.0%~97.0%之间,可替宁的平均回收率在90.0%~102.0%之间,RSD<5%。结论本方法简便、快速、准确,适用于被动吸烟人群头发中尼古丁和可替宁含量的测定。
Objective To establish a method for the determination of nicotine and cotinine in hair by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS). Methods The hair samples were completely digested with NaOH solution and extracted with dichloromethane + methanol (3 + 1). The mobile phase was eluted with 10 mmol / L ammonium acetate (containing 0.1% formic acid) - acetonitrile as mobile phase. Chromatography tandem mass spectrometry multiple reaction monitoring (MRM) mode determination, internal standard quantification. Results The regression equation of nicotine in the range of 2 ~ 200μg / L was y = 1.296 7x-2.379 9, r = 0.999 6; cotinine was in the range of 0.2 ~ 20μg / L and the regression equation was y = 1.099 2x -0.005 15, r = 0.999 9. With 3 times SNR, the detection limits of nicotine and cotinine were 0.01μg / g and 0.001μg / g respectively when the sample volume was 50 mg. The average recoveries of nicotine obtained by this method ranged from 75.0% to 97.0%, and the average recoveries of cotinine ranged from 90.0% to 102.0% with a RSD <5%. Conclusion This method is simple, rapid and accurate and suitable for the determination of nicotine and cotinine in the hair of passive smokers.