超高效液相色谱-串联质谱法快速测定吸烟者尿液中尼古丁和可替宁

doi:10.11973/lhjy-hx201911008

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理化检验-化学分册 ›› 2019, Vol. 55 ›› Issue (11) : 1287-1291. DOI: 10.11973/lhjy-hx201911008

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工作简报

超高效液相色谱-串联质谱法快速测定吸烟者尿液中尼古丁和可替宁

李晶¹, 梁梦洁², 刘欣¹, 王晋¹, 黄海涛¹, 许永¹, 李雪梅¹, 杨光宇¹, 孔维松¹, 杨叶昆¹

作者信息 +

Rapid Determination of Nicotine and Cotinine in Urine of Smokers by UHPLC-MS/MS

LI Jing¹, LIANG Mengjie², LIU Xin¹, WANG Jin¹, HUANG Haitao¹, XU Yong¹, LI Xuemei¹, YANG Guangyu¹, KONG Weisong¹, YANG Yekun¹

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文章历史 +

摘要

吸烟者尿液样品用自主研究开发设计的前处理萃取瓶处理，采用超高效液相色谱-串联质谱法快速测定萃取液中尼古丁和可替宁的含量。以Waters ACQUITY UPLC BEHHILIC色谱柱（50 mm×2.1 mm，1.7 μm）为固定相，以含0.1%（质量分数）氨水的甲醇（6+4）溶液为流动相，串联质谱中采用正离子模式监测。以D₄-尼古丁和D₃-可替宁为内标物，尼古丁和可替宁的线性范围均为20.0~2 000 μg·L^-1，检出限（3S/N）依次为5.7，3.7 μg·L^-1。在2.0，4.0，8.0 μg等3个浓度水平进行加标回收试验，回收率为93.6%~112%，测定值的日内相对标准偏差（n=7）为2.9%~3.4%，日间相对标准偏差（n=7）为3.2%~3.6%。

Abstract

The urine samples of smokers were prepared by a self-designed extraction vial. UHPLC-MS/MS was applied to the rapid determination of nicotine and cotinine in the extract. Waters ACQUITY UPLC BEHHILIC chromatographic column (50 mm×2.1 mm, 1.7 μm) was used as stationary phase, and methanol (6+4) solution[containing 0.1% (mass fraction) ammonia] was used as mobile phase; positive ionization was used in MS/MS. D₄-nicotine and D₃-cotinine were used as internal standards. Linearity ranges of nicotine and cotinine were found in the same range of 20.0-2 000 μg·L^-1, with detection limits (3S/N) of 5.7,3.7 μg·L^-1, respectively. Tests for recovery were made by standard addition method at the concentration levels of 2.0, 4.0, 8.0 μg. Values of recovery were in the range of 93.6%-112%, and values of intra-day RSDs (n=7) and inter-day RSDs (n=7) of determined values were in the range of 2.9%-3.4% and 3.2%-3.6%, respectively.

导出引用

李晶, 梁梦洁, 刘欣, 王晋, 黄海涛, 许永, 李雪梅, 杨光宇, 孔维松, 杨叶昆. 超高效液相色谱-串联质谱法快速测定吸烟者尿液中尼古丁和可替宁[J]. 理化检验-化学分册, 2019, 55(11): 1287-1291 https://doi.org/10.11973/lhjy-hx201911008

LI Jing, LIANG Mengjie, LIU Xin, WANG Jin, HUANG Haitao, XU Yong, LI Xuemei, YANG Guangyu, KONG Weisong, YANG Yekun. Rapid Determination of Nicotine and Cotinine in Urine of Smokers by UHPLC-MS/MS[J]. Physical Testing and Chemical Analysis Part B:Chemical Analgsis, 2019, 55(11): 1287-1291 https://doi.org/10.11973/lhjy-hx201911008

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