Gabr Raniah Q, Elsherbiny Marwa E, Somayaji Vishwa, Pollak P Timothy, Brocks Dion R
Faculty of Pharmacy and Pharmaceutical Sciences, University of Alberta, Edmonton, Canada.
Biomed Chromatogr. 2011 Oct;25(10):1124-31. doi: 10.1002/bmc.1581. Epub 2011 Feb 10.
A liquid chromatographic mass spectrometric (LC-MS) assay for the quantification of nicotine and cotinine in human specimens was developed. Human serum and urine (100 μL) were subjected to liquid-liquid extraction. For glucuronidated cotinine, serum was alkalinized and hydrolyzed before extraction. The dried samples were reconstituted and run using gradient flow reverse-phase liquid chromatography with MS detection. The ions utilized for quantification of nicotine, cotinine and milrinone (internal standard) were 162.8, 176.9 and 211.9 m/z, respectively. The mean recoveries were over 80% for cotinine and nicotine with excellent linearity between nominal concentrations and peak area ratios, over a wide concentration range. The percentage coefficient of variation and mean error of the inter- and intra-day validations were <15% for nicotine and cotinine. Analysis of serum from cardiac patients receiving amiodarone suggested that a number of patients were either active smokers or exposed to second-hand smoke. Significant concentrations of nicotine and cotinine were measured in the urine of a known smoking volunteer. The method was highly specific, sensitive and applicable as a tool in detecting and monitoring the passive exposure to tobacco smoke using small specimen volumes (0.1 mL).
开发了一种用于定量人体样本中尼古丁和可替宁的液相色谱-质谱(LC-MS)分析方法。人血清和尿液(100μL)进行液-液萃取。对于葡萄糖醛酸化的可替宁,血清在萃取前先碱化并水解。干燥后的样本复溶,采用梯度流动反相液相色谱结合质谱检测进行分析。用于定量尼古丁、可替宁和米力农(内标)的离子分别为162.8、176.9和211.9 m/z。可替宁和尼古丁的平均回收率超过80%,在较宽的浓度范围内,标称浓度与峰面积比之间具有良好的线性关系。尼古丁和可替宁日间和日内验证的变异系数百分比和平均误差均<15%。对接受胺碘酮治疗的心脏病患者的血清分析表明,许多患者要么是现吸烟者,要么接触过二手烟。在一名已知吸烟志愿者的尿液中检测到了显著浓度的尼古丁和可替宁。该方法具有高度特异性、灵敏性,适用于使用少量样本(0.1 mL)检测和监测被动吸烟暴露情况。