新型磁性氧化石墨烯-固相萃取-超高效液相色谱-串联质谱检测蔬菜中10种氨基甲酸酯类农药及其代谢物  

Determination of 10 Carbamate Pesticides and Its Metabolite in Vegetables Based on the Combination of Novel Magnetic Graphene Oxide Material-SPE and UPLC-MS/MS

作　　者：王小花 黄韡 苏阿龙 禹洁 赵生燕 张月胜 周佳 WANG Xiaohua;HUANG Wei;SU Along;YU Jie;ZHAO Shengyan;ZHANG Yuesheng;ZHOU Jia(Gansu Food Inspection and Research Institute,Lanzhou 730200,China)

机构地区：[1]甘肃省食品检验研究院,甘肃兰州730200

出　　处：《食品科技》2024年第9期316-324,共9页Food Science and Technology

基　　金：甘肃省市场监督管理局科研项目(SSCJG-SP-202103);甘肃省科技计划项目(23JRRA1709)。

摘　　要：文章通过化学共沉淀法制备得到磁性Fe_(3)O_(4)/GO,再引入对二氨基联苯得到胺化的磁性氧化石墨烯(Fe_(3)O_(4)/GO@DABP)。利用其吸附性和磁性,将其作磁固相萃取的吸附剂,与液相色谱-串联质谱法联用检测蔬菜中的10种氨基甲酸酯类农药及其代谢物。实验中探讨了不同萃取因素对萃取效率的影响,确定了最佳的液质条件、吸附剂用量、吸附时间、盐效应、洗脱试剂种类、洗脱剂体积。在最优的条件下建立了蔬菜中10种氨基甲酸酯类农药的磁性固相微萃取-液相色谱-串联质谱检测方法。实验结果表明,10种目标物的线性范围为1~100 ng/mL,相关系数R^(2)均不低于0.9990。检出限(LOD,S/N=3)范围为0.0128~0.08μg/kg,加标回收率为80.1%~101.3%,相对标准偏差为2.9%~7.4%。该方法准确度和精密度良好,该磁性氧化石墨烯复合材料能够应用于蔬菜中10种氨基甲酸酯类农药的检测。Magnetic Fe_(3)O_(4)/GO was prepared by chemical co-precipitation method,and then p-diaminobenzene was introduced to obtain aminated magnetic graphene oxide,(Fe_(3)O_(4)/GO@DABP).It was used as an adsorbent for magnetic solid phase microextraction due to its adsorbability and magnetism,and 10 kinds of carbamate pesticides and their metabolites in vegetables were detected by liquid chromatography-tandem mass spectrometry(LC-MS/MS).The effects of different extraction factors on extraction efficiency were discussed,and the optimal liquid chromatography-mass spectrometry conditions,adsorption material amount,adsorption time,salt effect,eluent type and eluent dosage were established.A magnetic solid phase extraction-liquid chromatography-tandem mass spectrometry method was established under the optimal conditions for the detection of carbamate pesticides in vegetables.The experimental results showed that the linear ranges of the 10 target compounds ranged from 1 ng/mL to 100 ng/mL,the correlation coefficients R^(2) were all not less than 0.9990,the limits of detection(LOD,S/N=3)ranged from 0.0128μg/kg to 0.08μg/kg,the recoveries ranged from 80.1%to 101.3%,the relative standard deviations ranged from 2.9%to 7.4%.The method demonstrated good accuracy and precision,the novel magnetic graphene oxide composite material can be applied to the detection of carbamate pesticides in vegetables.

关 键 词：磁性氧化石墨烯复合材料 液相色谱-串联质谱法 氨基甲酸酯农药 蔬菜 

分 类 号：TS207.53[轻工技术与工程—食品科学]