王孝钢 范津珲 江志训 刘彩飞

摘    要：為解决有机磷农药残留量检测分析过程中基质效应影响检测结果的问题，本研究以电喷雾（ESI）为离子源，正离子模式多级反应离子检测（MRM）方式，建立了一种灵敏度高、选择性强的基质校正液相色谱-串联质谱法（LC-MS/MS），以同时测定洋葱、葱、姜、蒜及韭菜中28种有机磷农药残留量。以洋葱为试材，优化选择了乙酸/乙腈（1：100Vol）+6 g氯化钠为最佳提取体系，并确定超声提取30 min、快速混匀器振荡1.5 min为最佳提取条件。利用该方法检测洋葱28种有机磷农药含量，在0.200～100 μg·L-1质量浓度范围内其与峰面积之间呈线性关系，相关系数为0.998 27～0.999 90;方法检出限0.06～0.89 μg·kg-1，定量限0.24～3.6 μg·kg-1;28种有机磷农药残留量在10.0，50.0，200 μg·kg-13个浓度水平的平均回收率为76.4%～102.6%，相对标准偏差为1.1%～9.0%。利用该方法检测葱、姜、蒜及韭菜中28种有机磷农药残留量在10 μg·kg-1浓度水平的平均回收率为74.7%～109.9%，相对标准偏差为0.61%～6.2%。综合而言，所建立的新方法能满足实际样品分析检测的要求。

关键词：液相色谱-串联质谱法;有机磷农药;洋葱;葱;姜;蒜;韭菜

中图分类号：0657.63;S481.8         文献标识码：A          DOI 编码：10.3969/j.issn.1006-6500.2021.12.012

Determination of 28 Organophosphorus Pesticide Residues in Onion， Scallion， Ginger， Garlic and Leek by LC/MS/MS

WANG Xiaogang1， FAN Jinhui1， Jiang Zhixun1， LIU Caifei2

（1. Qingdao Academy of Agricultural Sciences， Qingdao， Shandong 266109， China; 2. Agricultural and Rural Bureau of Jimo District， Qingdao， Shandong 266200， China）

Abstract： In order to solve the matrix effect in the detection process， the experiment developed a highly sensitive， selective， and matrix corrected LC-MS/MS method by electrospray ionization （ESI） as ion source and MRM in positive ion mode， which could simultaneously determine 28 organophosphorus pesticide residues of onion， scallion， ginger， garlic and leek. Using onion as material， the conditions of HPLC and MS for determination of 28 organophosphorus pesticides were optimized， the optimal extraction system were acetic acid /acetonitrile （1：100Vol） +6 g NaCl， and the optimal extraction process were 30 min of ultrasonic extraction and 1.5 min rapid mixer oscillation. The above method were used to detect  the 28 organophosphorus pesticides in onion， there was a good linear relationship between the organophosphorus pesticides content and peak area in the range of 0.200-100 μg·L-1， and the correlation coefficients were 0.998 27-0.999 90; the detection and quantitation limit were in the range of 0.06-0.89 μg·kg-1 and 0.24-3.6 g·kg-1， respectively; the recovery rate of 28 organophosphorus pesticides residues for 10， 50， 200 μg·kg-1 levels ranged from 76.4% to 102.6%， which the relative standard deviation were ranged from1.1% to 9.0%. The above method were used to detect the 28 organophosphorus pesticides residues in scallion， ginger， garlic， and leek， the recovery rate for 10 μg·kg-1 level were ranged from 74.7% to 109.9% ， which the relative standard deviation were ranged from 0.61% to 6.2%. Comprehensively， the new method could meet the requirements of actual sample analysis.

Key words： LC-MS/MS; organophosphorus pesticide residues; onion; scallion; ginger; garlic; leek

有机磷农药是一类广泛用于防治植物病虫害的高效广谱杀虫剂，同时对人畜也有较高的毒害性。在日常农产品检测中，常常在蔬菜、水果中能检测出有机磷农药残留。洋葱、葱、姜、蒜及韭菜等是一类具特殊香辛的鳞茎类蔬菜，该类蔬菜基质中含有大量的含硫化合物，对准确测定有机磷农药残留量的影响很大，易出现假阳性和假阴性，是农药残留检测公认的测定难题[1]。因此，研究洋葱、葱、姜、蒜及韭菜中多种有机磷残留检测技术具有十分重要的意义。……