摘要
建立了分子印迹固相萃取-超高效液相色谱-串联质谱法测定雪茄烟叶中4种烟草特有亚硝胺。样品经0.1mol/L乙酸铵溶液提取,分子印迹固相萃取柱净化,采用ACQUITYUPLCBEHC18色谱柱分离,以0.2mmol/L乙酸铵甲醇-乙酸铵溶液作为流动相进行梯度洗脱,在电喷雾离子源正离子模式,多反应监测模式下进行检测,以同位素内标法定量。4种烟草特有亚硝胺的质量浓度在1~200 ng/mL范围内与色谱峰面积线性关系良好,相关系数均大于0.99,检出限为1.00~2.25μg/kg。样品的平均回收率为95.67%~102.33%,测定结果的相对标准偏差1.18%~7.28%(n=6)。该方法灵敏度高、准确度高,适合雪茄烟叶中4种烟草特有亚硝胺的测定。
A molecular imprinting solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry method was established for the determination of 4 tobacco specific nitrosamines in cigar tobacco leaves.The samples were extracted by 0.1 mol/L ammonium acetate aqueous solution,purified by molecular-imprinted solid phase extraction column,separated by ACQUITY UPLC BEH C18 chromatographic column,and then gradient elution was performed with 0.2 mmol/L ammonium acetate methanol-ammonium acetate aqueous solution as mobile phase.The samples were detected in the positive ion mode of electrospray ion source and multi-reaction monitoring mode,and quantified by isotope internal standard method.The mass concentration of 4 nitrosamines specific in tobacco had a good linear relationship with the chromatographic peak area in the range of 1-200 ng/mL,the correlation coefficients were greater than 0.99,and the detection limits were 1.00-2.25μg/kg.The average recoveries were 95.67%-102.33%,and the relative standard deviations were 1.18%-7.28%(n=6).The method has high sensitivity and accuracy,which is suitable for the determination of nitrosamines specific to 4 kinds of tobacco in cigar leaves.
作者
陈伟祥
翟大成
徐万超
瞿长波
谢鑫
CHEN Weixiang;ZHAI Dacheng;XU Wanchao;QU Changbo;XIE Xin(YunNan Jiahui Testing Technology Co.,Ltd.,Kunming 650217,China)
出处
《化学分析计量》
CAS
2024年第11期46-51,共6页
Chemical Analysis And Meterage
关键词
超高效液相色谱-串联质谱法
雪茄烟
烟草特有亚硝胺
分子印迹固相萃取
ultra performance liquid chromatography-tandem mass spectrometry
cigar tobacco
tobacco specific nitrosamines(TSNAs)
molecularly imprinted solid phase extraction