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目的探讨建立溶剂去乳化分散液-液微萃取(dispersive liquid-liquid microextraction,DLLME)结合气相色谱-质谱法(gas chromatography-mass,GC/MS)测定尿液中尼古丁和可替尼的方法。方法考察GC/MS检测和DLLME条件。取5mL尿样,用NaOH调节pH至9.0,加入氯化钠振荡溶解后,取100μL三氯甲烷(含内标物喹啉)和1 000μL甲醇分别作为萃取剂和分散剂并混合,注入样液中使乳化分散,4 000r/min离心5min,弃上清,取1μL下层有机相进GC/MS分析。以DB-5毛细管色谱柱为分离柱,程序升温分离样液中的尼古丁和可替尼,离子监测(SIM)模式质谱检测和内标工作曲线法进行定量。结果尼古丁和可替尼在0.2~100ng/mL范围内线性良好,方法检出限分别为0.010ng/mL和0.022ng/mL,方法精密度(相对标准偏差)分别为8.2%和9.6%,加标回收率分别为92.0%~108.0%和83.0%~110.0%。结论本方法简单快速、灵敏准确,适用于尿液中尼古丁和可替尼的测定,能满足人群烟草暴露评价的需要。
OBJECTIVE: To establish a method for the determination of nicotine and cotinib in urine by solvent-emulsified liquid-liquid microextraction (DLLME) and gas chromatography-mass spectrometry (GC / MS). Methods Investigate GC / MS detection and DLLME conditions. Take 5mL urine sample, adjust the pH to 9.0 with NaOH, add sodium chloride oscillation and dissolve, take 100μL chloroform (containing internal standard quinoline) and 1000μL methanol as extractant and dispersant respectively, In the emulsion dispersed, 4 000r / min centrifugation 5min, the supernatant was discarded, take 1μL lower organic phase by GC / MS analysis. The DB-5 capillary column was used as the separation column, and the nicotine and cotinidine in the sample were separated by temperature program, and the ion monitoring (SIM) mode was used for mass spectrometry detection and internal standard curve method. Results The linearity of nicotine and cotinine in the range of 0.2-100 ng / mL was good. The detection limits were 0.010 ng / mL and 0.022 ng / mL, respectively. The precision (relative standard deviation) of the method was 8.2% and 9.6%, respectively The standard recoveries were 92.0% ~ 108.0% and 83.0% ~ 110.0%, respectively. Conclusion The method is simple, sensitive and accurate and suitable for the determination of nicotine and cotinidine in urine, which can meet the needs of tobacco exposure assessment in the population.