在线热脱附-GC/MS法检测人体尿液中烟碱及可替宁  

Quantifying nicotine and cotinine levels in human urine using automated thermal desorption-gas chromatography/mass spectrometry

作　　者：汪阳忠 李钢[1] 陶立奇 吴达[1] 刘百战[1] WANG Yangzhong;LI Gang;TAO Liqi;WU Da;LIU Baizhan(Technology Center,Shanghai Tobacco Group Co.,Ltd.,Shanghai 200082,China)

机构地区：[1]上海烟草集团有限责任公司技术中心

出　　处：《烟草科技》2019年第10期37-43,共7页Tobacco Science & Technology

摘　　要：为检测人体尿液中的烟碱及可替宁,建立了自动化的在线热脱附-气相色谱-质谱联用(GC/MS)方法。以水蒸气焙烧改性的SBA-15为吸附-脱附材料,结合GC/MS,自主设计了高效富集和在线快速分析尿液中烟碱及其代谢物可替宁的实验装置。结果表明:该装置实现了集样品的吸附、热脱附、进样、分析于一体的在线评价功能;选用700℃下水蒸气焙烧6h的SBA-15为吸附-脱附材料,可显著提高烟碱及可替宁分子的热脱附能力;烟碱及可替宁在质量浓度1~2000ng/mL范围内工作曲线具有良好的线性关系(R^2≥0.9995),方法回收率为97.28%~104.55%,相对标准偏差(RSD)为0.25%~3.18%;烟碱及可替宁的检测限分别为0.5和0.4ng/mL。该方法自动化程度高,分析速度快,适用于吸烟者尿液中烟碱及可替宁含量的分析。In order to quantify the nicotine and cotinine levels in human urine, an automatic online thermal desorption-gas chromatography/mass spectrometry (GC/MS) method was developed. By using steam-treated SBA-15 type mesoporous silica as the sorbent and coupling with GC/MS, a device was designed for the efficient enrichment and rapid online analysis of nicotine and its metabolite cotinine in urine. The results showed that the device realized the online sample adsorption, thermal desorption, injection and analysis. The SBA-15 type mesoporous silica modified with steam at 700 ℃ for 6 h significantly improved the thermal desorption of nicotine and cotinine. Calibration curves in the range of 1-2 000 ng/mL of the analytes were established with R2 higher than 0.999 5. The spiked recoveries of the analytes ranged from 97.28% to 104.55% with the relative standard deviations(RSDs)of 0.25%-3.18%. The limits of detections for nicotine and cotinine were 0.5 and 0.4 ng/mL, respectively. This method is highly automatic, rapid and suitable for the analysis of nicotine and cotinine in human urine samples.

关 键 词：吸烟者 尿液 烟碱 可替宁 GC/MS 改性SBA-15 热脱附 

分 类 号：TS416[农业科学—烟草工业]