Determination of 16 Carbamate Pesticide Residues in High-Sulfur Vegetables by UHPLC-MS/MS after Preparation of Sample with QuEChERS
摘 要
采用QuEChERS结合超高液相色谱-串联质谱法(UHPLC-MS/MS)测定了洋葱、葱、韭菜、蒜薹、生姜和大蒜等6种高硫蔬菜中16种氨基甲酸酯类农药残留量。样品用冷冻后的乙腈涡旋提取,用无水硫酸镁及氯化钠盐析,用无水硫酸镁、N-丙基乙二胺(PSA)和C18对上层提取物进行分散固相萃取净化,待测液在优化的仪器工作条件下测定。在色谱分离中,选择Waters ACQUITY UPLC BEH C18色谱柱作固定相,用不同比例的含0.1%(体积分数)甲酸的乙腈溶液(A)和0.1%甲酸溶液(B)为流动相进行梯度洗脱;采用电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式进行质谱分析。采用基质匹配标准溶液制作标准曲线,结果显示,16种农药的质量浓度均在一定的范围内与其对应的峰面积呈线性关系,检出限(3S/N)为0.1~20 μg·kg-1。对蒜薹进行3个浓度水平的加标回收试验,回收率为65.7%~112%,相对标准偏差(n=6)为1.5%~11%。按此方法分析了34批次高硫蔬菜,在其中2批洋葱中检出了乙霉威,其质量分数为0.040,0.178 mg·kg-1;1批生姜中检出仲丁威,其质量分数为0.092 mg·kg-1。
Abstract
A method based on UHPLC-MS/MS after preparation of sample with QuEChERS was developed for simultaneous determination of 16 carbamate pesticide residues in 6 high-sulfur vegetables, including onion, onionleek, Chinese chive, garlic scape, ginger and garlic. Samples were extracted with frozen acetonitrile and salted out with anhydrous magnesium sulfate and sodium chloride. The upper extract was purified by dispersion solid phase extraction with anhydrous magnesium, PSA and C18, the analytes were determined under the optimized working conditions of the instrument. In UHPLC analysis, Waters ACQUITYUPLC BEH C18 chromatographic column was adopted as stationary phase, and the mixed solution consisted of acetonitrile solution containing 0.1% formic acid (A) and 0.1% formic acid solution (B) with various ratios was used as mobile pahse for gradient elution. MS analysis was made under ESI+ and MRM mode. Matrix-matched standard solution series was prepared for making the standard curve, and results showed that the mass concentrations of 16 pesticides had linearity relationships with their respective peak areas in the definite ranges, with detection limits in the range of 0.1-20 μg·kg-1. Recovery test was made on garlic scape at the 3 concentration levels, giving recoveries in the range of 65.7%-112%, and RSDs (n=6) of the determined values were ranged from 1.5% to 11%. The proposed method was used for the analysis to the 34 batches of high-sulfur vegetable samples, diethofencarb was found in 2 batches of onions samples with mass fraction of 0.040, 0.178 mg·kg-1, and fenobucarb was detected in a batch of ginger sample with mass fraction of 0.092 mg·kg-1.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202101009
所属栏目 工作简报
基金项目
收稿日期 2020/2/20
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联系人作者周斌(362211547@qq.com)
备注杨坤,工程师,研究方向为食品质量与安全检测分析
引用该论文: YANG Kun,ZHANG Jianyang,ZHOU Bin. Determination of 16 Carbamate Pesticide Residues in High-Sulfur Vegetables by UHPLC-MS/MS after Preparation of Sample with QuEChERS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(1): 45~51
杨坤,张建炀,周斌. QuEChERS前处理结合超高液相色谱-串联质谱法测定高硫蔬菜中16种氨基甲酸酯类农药残留[J]. 理化检验-化学分册, 2021, 57(1): 45~51
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参考文献
【1】许文娟,王振刚,丁葵英,等.QuEChERS/液相色谱-串联质谱法测定5种蔬菜中17种氨基甲酸酯类农药的基质效应研究[J].分析测试学报, 2017,36(1):54-60.
【2】何华丽,徐小民,吕美玲,等.液相色谱-串联质谱法测定生姜中的氨基甲酸酯类农药及其代谢物残留[J].分析测试学报, 2014,33(2):197-202.
【3】张帆,张莹,黄志强,等.多壁碳纳米管固相萃取/超高效液相色谱-串联质谱测定茶油中12种氨基甲酸酯类农药[J].分析测试学报, 2019,38(4):411-416.
【4】周嘉诚,陈楠,黎小鹏,等.高效液相色谱法测定葡萄中8种氨基甲酸酯农药残留[J].现代农业科技, 2016,2016(8):117-118.
【5】陈建波,张颂函,马琳,等.高效液相色谱法测定农药产品中非法添加的限制性农药氨基甲酸酯的含量[J].理化检验-化学分册, 2019,55(1):68-72.
【6】卢忠魁,常海华,尚轶,等.反相高效液相色谱法测定生活饮用水中氨基甲酸酯农药残留[J].中国卫生检验杂志, 2015,25(21):3617-3619.
【7】于彦彬,谭丕功,曲璐璐,等.PSA分散固相萃取液相色谱柱后衍生荧光法测定蔬菜和水果中的13种氨基甲酸酯[J].分析试验室, 2009,28(11):97-101.
【8】王晓亮,毛卫中,汪新华,等.QuEchERs-高效液相色谱柱后衍生法测定茶叶中10种氨基甲酸酯类农药残留[J].食品工业科技, 2018,39(14):190-193.
【9】田宏哲,赵瑛博,周艳明.高效液相色谱-质谱法测定牛奶中6种氨基甲酸酯农药残留[J].食品科学, 2011,32(2):187-190.
【10】达晶,王钢力,曹进,等.QuEChERS-液相色谱-串联质谱法测定植物性食品中30种氨基甲酸酯类农药残留[J].色谱, 2015,33(8):830-837.
【11】王连珠,周昱,黄小燕,等.基于QuEChERS提取方法优化的液相色谱-串联质谱法测定蔬菜中51种氨基甲酸酯类农药残留[J].色谱, 2013,31(13):1167-1175.
【12】王泽锋,石玲,苏一兰,等.液质联用技术检测紫薯蓣中5种氨基甲酸酯农药的方法研究[J].食品工业科技, 2014,35(11):306-308.
【13】向平,沈敏,卓先义.液相色谱-质谱分析中的基质效应[J].分析测试学报, 2009,28(6):753-756.
【14】于杰,李晓玉,李淑娟,等.LCMSMS测定果蔬中氨基甲酸酯类农药的基质效应研究[J].食品研究与开发, 2013,34(23):41-44.
【15】李淑娟,于杰,高玉生,等.HPLC-MSMS测定果蔬中有机磷类农药的基质效应[J].食品工业科技, 2017,38(6):49-53.
【16】ZHOU Y, GUAN J, GAO W W, et al. Quantification and confirmation of fifteen carbamate pesticide residues by multiple reaction monitoring and enhanced product ion scan modes via LC-MS/MS QTRAP system[J]. Molecules, 2018,23(10):2481-2496.
【17】SHI Z H, LI Q, XU D, et al. Graphene-based pipette tip solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry for the analysis of carbamate pesticide residues in fruit juice[J]. Journal of Separation Science, 2016,39(22):4391-4397.
【18】ROBERTA S S, NAVICKIENE S. Multiresidue determination of carbamate, organophosphate, neonicotinoid, and triazole pesticides in roasted coffee using ultrasonic solvent extraction and liquid chromatography-tandem mass spectrometry[J]. Journal of AOAC International, 2019,102(1):33-37.
【2】何华丽,徐小民,吕美玲,等.液相色谱-串联质谱法测定生姜中的氨基甲酸酯类农药及其代谢物残留[J].分析测试学报, 2014,33(2):197-202.
【3】张帆,张莹,黄志强,等.多壁碳纳米管固相萃取/超高效液相色谱-串联质谱测定茶油中12种氨基甲酸酯类农药[J].分析测试学报, 2019,38(4):411-416.
【4】周嘉诚,陈楠,黎小鹏,等.高效液相色谱法测定葡萄中8种氨基甲酸酯农药残留[J].现代农业科技, 2016,2016(8):117-118.
【5】陈建波,张颂函,马琳,等.高效液相色谱法测定农药产品中非法添加的限制性农药氨基甲酸酯的含量[J].理化检验-化学分册, 2019,55(1):68-72.
【6】卢忠魁,常海华,尚轶,等.反相高效液相色谱法测定生活饮用水中氨基甲酸酯农药残留[J].中国卫生检验杂志, 2015,25(21):3617-3619.
【7】于彦彬,谭丕功,曲璐璐,等.PSA分散固相萃取液相色谱柱后衍生荧光法测定蔬菜和水果中的13种氨基甲酸酯[J].分析试验室, 2009,28(11):97-101.
【8】王晓亮,毛卫中,汪新华,等.QuEchERs-高效液相色谱柱后衍生法测定茶叶中10种氨基甲酸酯类农药残留[J].食品工业科技, 2018,39(14):190-193.
【9】田宏哲,赵瑛博,周艳明.高效液相色谱-质谱法测定牛奶中6种氨基甲酸酯农药残留[J].食品科学, 2011,32(2):187-190.
【10】达晶,王钢力,曹进,等.QuEChERS-液相色谱-串联质谱法测定植物性食品中30种氨基甲酸酯类农药残留[J].色谱, 2015,33(8):830-837.
【11】王连珠,周昱,黄小燕,等.基于QuEChERS提取方法优化的液相色谱-串联质谱法测定蔬菜中51种氨基甲酸酯类农药残留[J].色谱, 2013,31(13):1167-1175.
【12】王泽锋,石玲,苏一兰,等.液质联用技术检测紫薯蓣中5种氨基甲酸酯农药的方法研究[J].食品工业科技, 2014,35(11):306-308.
【13】向平,沈敏,卓先义.液相色谱-质谱分析中的基质效应[J].分析测试学报, 2009,28(6):753-756.
【14】于杰,李晓玉,李淑娟,等.LCMSMS测定果蔬中氨基甲酸酯类农药的基质效应研究[J].食品研究与开发, 2013,34(23):41-44.
【15】李淑娟,于杰,高玉生,等.HPLC-MSMS测定果蔬中有机磷类农药的基质效应[J].食品工业科技, 2017,38(6):49-53.
【16】ZHOU Y, GUAN J, GAO W W, et al. Quantification and confirmation of fifteen carbamate pesticide residues by multiple reaction monitoring and enhanced product ion scan modes via LC-MS/MS QTRAP system[J]. Molecules, 2018,23(10):2481-2496.
【17】SHI Z H, LI Q, XU D, et al. Graphene-based pipette tip solid-phase extraction with ultra-high performance liquid chromatography and tandem mass spectrometry for the analysis of carbamate pesticide residues in fruit juice[J]. Journal of Separation Science, 2016,39(22):4391-4397.
【18】ROBERTA S S, NAVICKIENE S. Multiresidue determination of carbamate, organophosphate, neonicotinoid, and triazole pesticides in roasted coffee using ultrasonic solvent extraction and liquid chromatography-tandem mass spectrometry[J]. Journal of AOAC International, 2019,102(1):33-37.
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