作者：张瑶1, 马桂娟1, 高琳1, 王紫昕1, 吴龙国2
作者单位：1. 宁夏食品检测研究院（国家市场监管重点实验室（枸杞和葡萄酒质量安全）），宁夏 银川 750021;
2. 宁夏大学，宁夏 银川 750021
关键词：固相萃取;气相色谱串联质谱法;黄瓜;农药残留
摘要：
该文利用气相色谱串联质谱法，结合固相萃取技术建立黄瓜中62种农药残留检测方法。样品提取后，经Envi-18柱及Envi-Carb柱及Sep-Pak柱串联柱净化后，浓缩氮吹近干，正己烷定容后，采用气相色谱-质谱联用法测定，外标法定量。62种农药在基质中的线性范围良好；以三个添加水平测定样品的回收率和RSD，加标回收率均在60.0%～120.0%之间，相对标准偏差为1.5%～15.3%，该方法准确、高效、灵敏，且净化效果好，为检测黄瓜中目标物提供参考。该方法可以满足一般实验室检测需求，也为其他果蔬中农药残留检测提供方法借鉴。
Determination of 62 pesticide residues in cucumber by GC-MS combined with solid phase extraction technology
ZHANG Yao1, MA Guijuan1, GAO Lin1, WANG Zixin1, WU Longguo2
1. Ningxia Food Testing and Research Institute (Key Laboratory of Quality and Safety of Wolfberry and Wine for State Administration For Market Regulation), Yinchuan 750021, China;
2. Ningxia University, Yinchuan 750021, China
Abstract: In this paper, a method for simultaneous determination of 62 pesticide residues in cucumber by gas chromatography tandem mass spectrometry combined with solid phase extraction was established. After extraction, the samples were purified by ENvi-18 column, ENvi-Carb column and SEP-PAK column, and the concentrated nitrogen was blown nearly dry. After volume determination of n-hexane, the samples were determined by gas chromatography- mass spectrometry and quantified by external standard method. The linear range of 62 pesticides in the substrate was good, and the detection limit reached the current pesticide residue limit standard in China.The recovery rate and RSD of the samples were measured at three additive levels. The recoveries of most pesticide compounds were between 60.0% and 120.0%, and the relative standard deviation was between 1.5% and 15.3%. The method is accurate, efficient, sensitive, and has good purification effect. It can be used as a reference for the detection of target compounds in cucumber. which can meet the actual needs of general laboratory testing, and also provides a method for the detection of pesticide residues in other fruits and vegetables.
Keywords: solid phase extraction technology;gas chromatography tandem mass spectrometry;cucumber;pesticide residues
2022, 48(9):63-70 收稿日期: 2021-08-08;收到修改稿日期: 2021-10-26
基金项目: 宁夏青年科技人才托举工程（TJGC2021075）
作者简介: 张瑶（1989-），女，宁夏银川市人，工程师，硕士，主要从事食品检测方向
参考文献
[1] 张子伦. 浅析农产品农药残留检测研究技术[J]. 农业开发与装备, 2020, 11: 100-101
[2] 马新耀, 王静, 朱九生. 山西省黄瓜农药残留检测及膳食摄入风险评估[J]. 生态毒理学报, 2020, 15(5): 333-344
[3] 王烽凡, 路峰. 高效液相色谱法检测黄瓜中的农药残留[J]. 现代农业科技, 2020, 5: 100
[4] 安静. 全自动固相萃取-气相色谱质谱法监测地表水中的5种有机磷类农药残留量[J]. 中国测试, 2019, 45(11): 61-65
[5] 孙志高, 盛冉, 郝静梅, 等. QuEChERS-高效液相色谱法检测柑桔中毒死蜱、吡虫啉和残杀威农残[J]. 食品与机械, 2017, 33(6): 68-72
[6] 兰丰, 姚杰, 周先学, 等. QuEChERS-超高效液相色谱-串联质谱法测定果蔬中螺虫乙酯、丁醚脲及代谢物残留[J]. 农药学学报, 2019, 21(2): 219-226
[7] 覃国新, 劳水兵, 莫仁甫, 等. 通过式固相萃取净化/超高效液相色谱-串联质谱法测定黄瓜、番茄及豇豆中的克百威与涕灭威残留[J]. 分析测试学报, 2019, 38(8): 967-972
[8] 宋梓豪, 张金振, 周欣欣, 等. QuEChERS-高效液相色谱-串联质谱法测定蜜蜂及蜂产品中5种农药及氟虫腈代谢物残留[J]. 农药, 2021, 60(5): 347-351
[9] 林海丹, 谢守新, 王岚, 等. 超高效液相色谱串联质谱法测定果蔬中13种植物生长调节剂残留量[J]. 广东农业科学, 2015, 42(9): 82-87
[10] 黄绍军, 杜萍, 杨俊, 等. 固相萃取-气相色谱-串联质谱法检测丽江玛咖中41种有机氯和菊酯类农药残留[J]. 食品科学, 2020, 41(16): 307-313
[11] 韩梅, 侯雪, 邱世婷, 等. QuEChERS-气相色谱-串联质谱法测定蔬菜中48种农药残留[J]. 中国测试, 2020, 46(5): 65-71+76
[12] PLANQUE M, AMOULD T, DELAHAUT P, et al. Development of a strategy for the quantification of food allergens in several food products by mass spectrometry in a routine laboratory[J]. Food Chem, 2019, 274: 35-45
[13] 钟志凌, 唐吉旺. 基于QuEChERS净化-气相色谱法同时测定蔬菜中6种有机磷类农药残留[J]. 分析测试技术与仪器, 2019, 25(1): 22-27
[14] 辛平, 徐银萍, 成娟, 等. 气质联用法(GC-MS)测定水果中农药残留含量[J]. 林业科技通讯, 2015, 9: 59-61
[15] 张群, 马晨, 秦安丽, 等. QuEChERS-气相色谱-串联质谱法同时测定豇豆中6种菊酯农药残留[J]. 中国测试, 2021, 47(2): 63-67
[16] 周秀玲. 优化的QuEChERS-UPLC-MS/MS法检测57种农药在黄瓜中的残留[D]. 泰安：山东农业大学, 2019.
[17] 黎宙, 陈辉, 周斌. 分散液液微萃取-气相色谱-串联质谱法测定黄瓜中9种农药的残留量[J]. 理化检验(化学分册), 2021, 57(2): 179-182
[18] 张志龙, 王雪娇, 李晓东, 等. QuEChERS萃取结合气相色谱串联三重四级杆质谱法同时测定黄瓜中15种农药残留[J]. 中国食品工业, 2021(1): 51-53
[19] 白国涛, 刘来俊, 盛万里, 等. QuEChERS-气相色谱-串联质谱法测定黄瓜中10种农药残留[J]. 农药学学报, 2019, 21(1): 89-96
[20] 张瑶, 吴龙国, 马桂娟, 等. 气相色谱—串联质谱结合固相萃取技术同时测定番茄和黄瓜中10种杀菌剂[J]. 食品与机械, 2020, 36(7): 67-71
