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(50mm×2.1mm,1.7μm)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 000μg·L^-1,检出限(3S/N)依次为5.7,3.7μg·L^-1。在2.0,4.0,8.0μg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%。
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,1.7μm)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 000μg·L^-1,with detection limits(3 S/N)of 5.7,3.7μg·L^-1,respectively.Tests for recovery were made by standard addition method at the concentration levels of 2.0,4.0,8.0μg.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.
作者
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
LI Jing;LIANG Mengjie;LIU Xin;WANG Jin;HUANG Haitao;XU Yong;LI Xuemei;YANG Guangyu;KONG Weisong;YANG Yekun(Technology Center,China Tobacco Yunnan Industrial Co.,Ltd.,Kunming 650106,China;School of Pharmacy,Kunming Medical University,Kunming 650504,China)
出处
《理化检验（化学分册）》
CAS
CSCD
北大核心
2019年第11期1287-1291,共5页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
云南中烟工业有限责任公司科研项目(2018JC09)
