头发中尼古丁和可替宁的超高效液相色谱-串联质谱测定法

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,RSD5%。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。

Determination of nicotine and cotinine in hair by ultra high performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for the determination of nicotine and cotinine in hair by ultra high performance liquid chromatography-tandem mass spectrometry (UPLC-MS-MS).Methods The hair samples were digested with NaOH solution and extracted with a mixed solvent dichloromethane-methanol (V∶V=3∶1).The nicotine and cotinine were separated with acetonitrile and 10 mmol/L ammonium acetate(containing 0.1％ formic acid,V∶V) aqueous solution as mobile phase for gradient elution,determined by UPLC-MS-MS in the multiple-reaction monitoring (MRM) mode and quantified by internal standard.Results In the range of 2-200 μg/L,the correlative regression equation of nicotine was y=1.296 7x-2.379 9,r=0.999 6;In the range of 0.2-20 μg/L,the correlative regression equation of cotinine was y=1.099 2x-0.005 15,r=0.999 9.The spiked recoveries were 75.0％-97.0％ for nicotine (RSD＜5％) and 90.0％-102％ for cotinine (RSD＜5％).The limits of detection were 0.01 μg/g for nicotine and 0.001 μg/g for cotinine invovled in the sample amount of 50 mg.Conclusion The method is simple,rapid,sensitive,accurate and applicable to the determination of nicotine and cotinine in hair of passive smoking people.