超临界流体色谱-串联质谱分离和测定烟草烯酰吗啉顺反异构体  

Determination of stereoisomers of dimethomorph in tobacco by supercritical fluid chromatography coupled with tandem mass spectrometry

作　　者：杨飞[1] 纪元 崔浩哲 王颖[1] 刘珊珊[1] 邓惠敏[1] 范子彦[1] 边照阳[1] 唐纲岭[1] 李中皓[3] YANG Fei;JI Yuan;CUI Haozhe;WANG Ying;LIU Shanshan;DENG Huimin;FAN Ziyan;BIAN Zhaoyang;TANG Gangling;LI Zhonghao(China National Tobacco Quality Supervision and Test Center,Zhengzhou 450001,China;School of Chemistry,Biology and Material Engineering,Suzhou University of Science and Technology,Suzhou 215009,Jiangsu,China;Zhengzhou Tobacco Research Institute of CNTC,Zhengzhou 450001,China)

机构地区：[1]国家烟草质量监督检验中心,郑州450001 [2]苏州科技大学化学生物与材料工程学院,江苏省215009 [3]中国烟草总公司郑州烟草研究院,郑州450001

出　　处：《烟草科技》2021年第6期42-49,共8页Tobacco Science & Technology

摘　　要：为实现烟草烯酰吗啉顺反异构体的立体选择性分离和测定,研究建立了超临界流体色谱-串联质谱(SFC-MS/MS)快速分离和测定烟草中烯酰吗啉顺反异构体的方法。样品经QuEChERS方法提取净化后,在Chiralcel OD-3色谱柱上以CO2-甲醇为流动相,流速为2.0 mL/min,采用基质匹配标准工作曲线进行定量分析。结果表明:①该方法可以快速实现(E)-(/Z)-烯酰吗啉异构体的基线分离,分离时间仅为5 min。②在各异构体质量分数为0.02、0.20和2.00 mg/kg水平下,各异构体的回收率为87.3%~102.3%,日间相对标准偏差(RSD)为3.3%~5.9%。在烯酰吗啉异构体浓度为2~100 ng/mL范围内,烟草基质中两种异构体的线性关系良好(R^(2)≥0.9943),检出限(LOD)和定量限(LOQ)分别为0.006~0.008和0.021~0.026 mg/kg。③采用该方法检测10个烟草实际样品,仅在1个样品中检出(E)-烯酰吗啉(1.18 mg/kg)和(Z)-烯酰吗啉(1.22 mg/kg)。该方法快速、环保、稳定、可靠,适用于烟草中烯酰吗啉异构体的立体选择性测定。In order to achieve the stereoselective separation and determination of stereoisomers of dimethomorph in tobacco,a method coupled supercritical fluid chromatography with tandem mass spectrometry(SFC-MS/MS)was developed to quickly separate and determine the stereoisomers of dimethomorph.Tobacco samples were extracted and purified by QuEChERS method,then the dimethomorph stereoisomers were well separated on a Chiralcel OD-3 column with CO2-methanol as the mobile phase at the flow rate of 2 mL/min.Matrix matching standard working curve was used to conduct quantitative analysis.The results showed that:(1)The stereoisomers of dimethomorph reached baseline separation,and the separation time was only 5 minutes.(2)At the mass fractions of 0.02,0.20 and 2.00 mg/kg,the recoveries of two isomers were in the range of 87.3%-102.3%with the inter-day relative standard deviations(RSDs)of 3.3%-5.9%.Good coefficients of determination(R2≥0.9943)were achieved for two isomers over the isomers concentration range of 2-100 ng/mL in tobacco.The limits of detection(LODs)and limits of quantification(LOQs)for two isomers were 0.006-0.008 and 0.021-0.026 mg/kg respectively.(3)Ten tobacco samples were tested by this method,and(E)-dimethomorph(1.18 mg/kg)and(Z)-dimethomorph(1.22 mg/kg)were detected only in one sample.This method is fast,environmentally friendly,stable,reliable,and suitable for the stereoselective determination of dimethomorph isomers in tobacco.

关 键 词：烟草 烯酰吗啉 立体选择性分离 立体异构体 超临界流体色谱 串联质谱 

分 类 号：TS411.1[农业科学—烟草工业]