高效液相色谱-四极杆飞行时间质谱技术非靶向快速筛查荔枝花、蜂巢和蜂蜜中农药

doi:10.7506/spkx1002-6630-20200409-126

食品科学 ›› 2021, Vol. 42 ›› Issue (20): 310-315.doi: 10.7506/spkx1002-6630-20200409-126

高效液相色谱-四极杆飞行时间质谱技术非靶向快速筛查荔枝花、蜂巢和蜂蜜中农药

王思威，孙海滨，刘艳萍，曾广丰，王潇楠，常虹，曾鑫年

（1.华南农业大学广东省昆虫行为调控工程技术研究中心，广东广州 510642；2.广东省农业科学院植物保护研究所，广东省植物保护新技术重点实验室，广东广州 510640；3.广东检验检疫技术中心，广东广州 510623）

出版日期:2021-10-25 发布日期:2021-11-12
基金资助:
广东省乡村振兴战略专项（403-2018-XMZC-0002-90）；国家荔枝龙眼产业技术体系项目（CARS-32-16）；广州市科技计划项目（202102080338）；广东省农业科学院院长基金项目（201929；202026）

Rapid Non-targeted Screening of Pesticide Residues in Litchi Flower, Hive and Honey by High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

WANG Siwei, SUN Haibin, LIU Yanping, ZENG Guangfeng, WANG Xiaonan, CHANG Hong, ZENG Xinnian

(1. Guangdong Engineering Research Center for Insect Behavior Regulation, South China Agricultural University, Guangzhou 510642, China; 2. Guangdong Provincial Key Laboratory of High Technology for Plant Protection, Institute of Plant Protection, Guangdong Academy of Agricultural Sciences, Guangzhou 510640, China; 3. Guangdong Inspection and Quarantine Technology Center, Guangzhou 510623, China)

Online:2021-10-25 Published:2021-11-12

摘要/Abstract

摘要： 利用高效液相色谱-四极杆飞行时间质谱结合QuEChERS前处理技术，建立荔枝花、蜂巢和蜂蜜中未知农药残留的非靶向快速筛查方法。样品均由乙腈溶液提取，经无水硫酸镁、N-丙基乙二胺和十八烷基键合硅胶吸附剂净化，采用Xbridge BEH C18色谱柱分离，以甲酸溶液-乙腈为流动相进行梯度洗脱，在电喷雾离子源、化学电离源和正反监测模式条件下进行检测。利用目标化合物特征离子的精确质量数、同位素匹配、二级碎片信息和保留时间进行数据库匹配，筛查可疑未知农药，在Targeted MS/MS模式下，通过相应碰撞能量下的离子碎片信息进一步确证，以基质匹配标准溶液法定量。结果显示：共计筛选出嘧菌酯、吡唑醚菌酯及其代谢物BF 500-3、苯醚甲环唑、多菌灵、毒死蜱、除虫脲和灭幼脲8 种农药，在1～1 000 μg/L范围内线性关系良好，相关系数r2均大于0.99，方法的检出限为0.03～0.50 μg/kg，定量限为0.4～0.8 μg/kg。8 种农药在荔枝花、蜂巢和蜂蜜中的平均加标回收率为80%～96%，相对标准偏差为1.2%～6.1%。该法快速、简便、灵敏，可用于荔枝花、蜂巢和蜂蜜样品中未知农药的筛查和鉴定。

关键词: 荔枝花、蜂巢和蜂蜜；高效液相色谱-四极杆飞行时间质谱；筛查；农药

Abstract: An analytical method using QuEChERS (quick, easy, cheap, effective, rugged and safe) pretreatment combined with high performance liquid chromatography-quadrupole-time of flight mass spectrometry (HPLC-Q-TOF-MS) was developed for the rapid non-targeted screening of unknown pesticide residues in litchi flower, hive and honey. The samples were extracted with acetonitrile-water, cleaned up with a mixture of anhydrous magnesium sulfate, N-propyl ethylene diamine (PSA) and octadecyl (C18) sorbent, separated on an Xbridge BEH C18 column by gradient elution using a mobile phase consisting of formic acid in water and acetonitrile, and detected using both electrospray ionization (ESI) and atmospheric pressure chemical ionization (APCI) under the positive and negative ion modes. Screening for unknown compounds suspected of being pesticides were carried out through database matching with the exact mass, isotopic distribution, secondary fragmentation information and retention time of the characteristic ions of the target compounds, and in the targeted MS/MS mode, the selected compounds were confirmed based on the ion fragment information at each collision energy. The analytes were quantified by using matrix-matched standard solutions. The results showed that eight pesticides (including azoxystrobin, pyraclostrobin and its metabolite BF 500-3, difenoconazole, carbendazim, chlorpyrifos, diflubenzuron and chlorbenzuron) were screened out. The calibration curves for these analyes had good linearity in the range of 1–1 000 μg/L with correlation coefficients (r2) above 0.99. The limits of detection were 0.03–0.50 μg/kg and the limits of quantification were 0.4–0.8 μg/kg. The average spiked recoveries of the pesticides in litchi flower, hive and honey samples were 80%–96% with relative standard deviations (RSDs) of 1.2%–6.1%. The developed method is quick, easy, sensitive and suitable for the rapid screening and identification of pesticide residues in litchi flower, hive and honey.

Key words: litchi flower, hive and honey; high performance liquid chromatography-quadrupole-time of flight mass spectrometry; screening; pesticide

中图分类号:

O658

王思威，孙海滨，刘艳萍，曾广丰，王潇楠，常虹，曾鑫年. 高效液相色谱-四极杆飞行时间质谱技术非靶向快速筛查荔枝花、蜂巢和蜂蜜中农药[J]. 食品科学, 2021, 42(20): 310-315.

WANG Siwei, SUN Haibin, LIU Yanping, ZENG Guangfeng, WANG Xiaonan, CHANG Hong, ZENG Xinnian. Rapid Non-targeted Screening of Pesticide Residues in Litchi Flower, Hive and Honey by High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry[J]. FOOD SCIENCE, 2021, 42(20): 310-315.

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高效液相色谱-四极杆飞行时间质谱技术非靶向快速筛查荔枝花、蜂巢和蜂蜜中农药

Rapid Non-targeted Screening of Pesticide Residues in Litchi Flower, Hive and Honey by High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry

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