高效液相色谱串联质谱法快速测定烟草中抑芽丹农药残留量  

Rapid Method for Determination of Maleic Hydrazide Residue in Tobacco with High Performance Liquid Chromatography-tandem Mass Spectrometry

作　　者：谢碧红 杨诗珍 Xie Bihong;Yang Shizhen(School of Electronic Information and Electrical Engineering Shanghai Jiaotong University,Shanghai 200241;Intertek Testing Services Ltd.,Shanghai 200233,China)

机构地区：[1]上海交通大学电子信息与电气工程学院,上海200241 [2]上海天祥质量技术有限公司,上海200233

出　　处：《广东化工》2022年第4期200-203,共4页Guangdong Chemical Industry

摘　　要：本文通过比较研究不同提取溶剂,不同提取参数,不同色谱柱条件及质谱参数,在YC/T 570-2018基础上优化前处理和仪器分析方法,建立一种高效液相色谱串联质谱法(HPLC-MS/MS)快速测定烟草中抑芽丹农药残留的方法。烟草样品经1%甲酸甲醇超声振荡提取10 min,提取液经PTFE膜过滤,氘代抑芽丹内标法定量,高效液相色谱串联质谱分析。结果表明,抑芽丹基质匹配工作曲线在0.1~10.0μg/mL,线性良好(R^(2)>0.995),方法定量限(S/N=10)为0.88 mg/kg。添加标准品2 mg/kg,10 mg/kg,80 mg/kg低、中、高三个浓度,回收率在94.1%~102.2%之间,相对标准偏差(RSD)范围3.1%~5.1%。采用本方法进行检测,具有前处理简便,快速,定量分析准确,灵敏度高,适用于大批量烟草样品中抑芽丹农药残留的快速分析。This study establish a rapid method of determination for maleic hydrazide by high liquid chromatography tandem mass spectrum in tobacoo,which optimized the sample pretreatment and instrument analysis method based on YC/T 570-2018,by study different extraction solvents,different extraction parameters,different chromatography columns and mass spectrum parameters.1%formic in methanol as an extracting solution was added to the sample by ultrasonic oscillation for 10 min,with maleic hydrazide-d;as an internal standard,about 1 mL of the supernatant portion of extracting solution was filtered by PTFE membrane and analyzed by HPLC-MS/MS.The results showed that the matrix-matched calibration curve range have good linearity in 0.1~10.0μg/mL with R^(2)>0.995,the limit of quantification (LOQ,S/N=10) was 0.88 mg/kg.The recoveries were 94.1%~102.2%with RSD of 3.1%~5.1%at three spike levels.The method was simple,rapid,accurate and sensitive,and suitable for the determination of maleic hydrazide residues in large quantities of tobacco samples.

关 键 词：烟草 抑芽丹 高效液相色谱串联质谱 农药残留 快速测定 

分 类 号：O65[理学—分析化学]