番茄、黄瓜及土壤中杀虫单总残留量的超高效液相色谱-电喷雾串联质谱检测  

Determination of monosultap total residues in tomato,cucumber and soil by ultra-performance liquid chromatographytandem mass spectrometry

作　　者：田春霞[1] 兰美静 马友宁 杨梅[1] 李舒盈 桂文君[1] 朱国念[1] 

机构地区：[1]浙江大学农药与环境毒理研究所,杭州310029

出　　处：《农药学学报》2014年第2期174-178,共5页Chinese Journal of Pesticide Science

摘　　要：建立了番茄、黄瓜及土壤中杀虫单残留的超高效液相色谱一电喷雾串联质谱（UPLC-MS／MS）检测方法。先将杀虫单在碱性条件下水解成沙蚕毒素，经乙醚液一液分配后用甲醇定容，采用UPLC-MS／MS法测定沙蚕毒素浓度，最后再折算成杀虫单的残留量。结果表明：在1～500μg／L范围内，杀虫单质量浓度与峰面积呈良好的线性关系，相关系数均大于0．99；仪器检出限（LOD）分别为0．213μg／kg（番茄）、0．212μg/kg（黄瓜）和0．172μg/kg（土壤），定量限（LOQ）分别为0．710μg／kg（番茄）、0．707μg／kg（黄瓜）和0．573μg/kg（土壤）；对于番茄、黄瓜及土壤样品，10、100和500μg／kg3个水平的添加回收率试验结果显示，方法的平均回收率在79％～101％之间，相对标准偏差（RSD）为6．6％～16％。该方法可用于番茄、黄瓜及土壤中杀虫单残留量检测。An analytical method was developed for residue determination of monosultap in tomato, cucumber and soil samples by ultra-performance liquid chromatography-electrospray tandem mass spectrometry （UPLC-MS/MS）. Firstly, monosultap was hydrolyzed to nereistoxin under alkaline condition. Then, after liquid-liquid partition with ether, the organic layer was evaporated and restructed in methanol. The formed nereistoxin was detected by UPLC-MS/MS, and the residue of monosultap could be calculated accordingly. Results showed good linearity ranging from 1 to 500 μg/L with correlation coefficients higher than 0.99; the limit of detection （LOD） was 0. 213 μg/kg （tomato matrix）, 0. 212 μg/kg （cucumber matrix） and 0. 172 μg/kg （soil matrix）, and the limit of quantification （LOQ） was 0. 710 p.g/kg （tomato matrix）, 0. 707 p.g/kg （cucumber matrix） and 0. 573 μg/kg （ soil matrix）. For tomato, cucumber and soil samples, average recoveriesranged from 79% to 101% at spiked level 10,100 and 500 μg/kg, and the relative standard deviations （RSD） was between 6.6% and 16%. The developed method is suitable for determination of monosultap total residues in tomato, cucumber and soil samples.

关 键 词：杀虫单 沙蚕毒素 超高效液相色谱-串联质谱 残留 黄瓜 番茄 土壤 

分 类 号：O657.63[理学—分析化学]