QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留
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摘要
目的:建立并应用QuEChERS结合液相色谱-串联质谱法测定食用菌中13种农药残留。方法:样品5.0 g用乙腈-水(4∶1) 15 m L超声提取,经N-丙基乙二胺(PSA) 30.0 mg和无水硫酸镁15.0 mg分散固相萃取吸附剂净化。使用HSS T3色谱柱,0.1%甲酸和乙腈为流动相梯度洗脱。质谱采用电喷雾正离子源和多反应监测模式。结果:13种农药的质量浓度在0.5～200μg/L范围内与峰面积呈良好的线性关系,检出限(S/N=3) 0.03～0.3μg/kg。加标回收率84.3%～102%,相对标准偏差(n=6) 2.8%～6.3%。结论:该方法可用于食用菌中13种农药残留的检测。
Objective: Determination of thirteen pesticides in edible mushrooms by Qu ECh ERS with UPLC MS/MS.Methods: 5.0 g sample was extracted ultrasonically for 5 min with 15 m L of 4∶ 1 acetonitrile and water.The extract was purified by N-propyl ethylenediamine( PSA) 30.0 mg,anhydrous Magnesium sulfate 15.0 mg dispersive solid-phase extraction adsorbent.The purified solution was separated by UPLC using HSS T3 column,0.1% formic acid and acetonitrile as mobile phase in gradient elution.Positive ESI and MRM were adopted in MS analysis. Results: Linear relationships were found between the peak area and the mass concentration of 13 pesticides within 0.5 ～ 200 μg/L. With detection limits( S/N = 3) in the range of 0.03 ～ 0.3 μg/kg,recovery rates obtained by standard addition method ranged from 84.3% to 102% and RSDs( n = 6) were in the range of 2.8%～6.3%.Conclusion: The proposed method was successfully applied to the detection of 13 pesticides in mushrooms.
Objective: Determination of thirteen pesticides in edible mushrooms by Qu ECh ERS with UPLC MS/MS.Methods: 5.0 g sample was extracted ultrasonically for 5 min with 15 m L of 4∶ 1 acetonitrile and water.The extract was purified by N-propyl ethylenediamine( PSA) 30.0 mg,anhydrous Magnesium sulfate 15.0 mg dispersive solid-phase extraction adsorbent.The purified solution was separated by UPLC using HSS T3 column,0.1% formic acid and acetonitrile as mobile phase in gradient elution.Positive ESI and MRM were adopted in MS analysis. Results: Linear relationships were found between the peak area and the mass concentration of 13 pesticides within 0.5 ～ 200 μg/L. With detection limits( S/N = 3) in the range of 0.03 ～ 0.3 μg/kg,recovery rates obtained by standard addition method ranged from 84.3% to 102% and RSDs( n = 6) were in the range of 2.8%～6.3%.Conclusion: The proposed method was successfully applied to the detection of 13 pesticides in mushrooms.
引文
[1]邱良妙,刘其全,赵建伟,等.4种杀虫剂对蘑菇迟眼蕈蚊的药效及其对双孢蘑菇的安全性评价[J].热带作物学报,2016,25(8):1540-1546.
[2]魏畅,傅红,郑俊超,等.QuECHERS-液质联用同步检测蘑菇中多菌灵等3种杀菌剂残留[J].中国食品学报,2016,6(11):189-195.
[3]张其才,董茂锋,宋卫国,等.超高效液相色谱法检测啶虫脒在工厂化双孢蘑菇栽培中的残留[J].农药学学报,2016,17(3):373-379.
[4]李琴,朱科学,周惠明.固相微萃取-气相色谱-质谱及气相色谱嗅闻技术分析双孢蘑菇汤的风味活性物质[J].食品科学,2011,22(16):300-304.
[5]王雪平,闫凯.固相萃取-气相色谱-质谱法测定饮用水中15种农药残留量[J].理化检验(化学分册),2017,53(4):437-441.
[6]侯雪,韩梅,邱世婷,等.改进的Qu ECh ERS气相色谱-串联质谱法测定草莓中21种杀菌剂残留[J].农药学学报,2017,11(1):46-52.
[7]程寿峰,魏绍峰,王兴宁,等.气相色谱-质谱法测定大米中15种苯氧羧酸类除草剂的残留量[J].理化检验(化学分册),2017,53(11):1281-1285.
[8]李婵君,李柱梅,秦喜玲,等.液相色谱-串联质谱法测定水产品中磺胺类及喹诺酮类药物残留量[J].理化检验(化学分册),2017,23(5):527-531.
[9]Elisa Helena da Costa Morais,Carol Hollingworth Collins,Isabel Cristina Sales Fontes Jardim.Pesticide determination in sweet peppers using Qu ECh ERS and LC-MS/MS[J].Food Chemistry,2018(249):77-83
[10]李继革,王玉飞,施家威,等.固相萃取-气相色谱-串联质谱法测定水果中11种三唑类杀菌剂[J].色谱,2012,6(03):262-266.
[11]Ferreira J A,Ferreira J M S,Talamini V,et al.Determination of pesticides in coconut(Cocos nucifera Linn.)water and pulp using modified Qu ECh ERS and LC-MS/MS[J].Food Chemistry,213(2016):616-624
[12]谢建军,陈捷,李菊,等.改良Qu ECh ERS法结合气相色谱串联质谱测定果蔬中20种杀菌剂[J].食品安全质量检测学报,2013,4(1):82-88.
[13]彭芳,雷美康,徐佳文,等.QuEChERS净化-超高效液相色谱-串联质谱法测定柑橘中7种保鲜剂的残留量[J].理化检验(化学分册),2016,52(9):1007-1010.
[14]Zhan Xiu-ping,Ma Lin,Huang Lan-qi,et al.The optimization and establishment of Qu ECh ERS-UPLC-MS/MSmethod for simultaneously detecting various kinds of pesticides residues in fruits and vegetables[J].Journal of Chromatography B,2017(1060):281-290.
[15]Pastor-Belda M,Garrido I,Campillo N,et al.Combination of solvent ext.ractants for dispersive liquid-liquid micro-extraction of fungicides from water and fruit samples by liquid chromatography with tandem mass spectrometry[J].Food Chemistry,2017(233):69-76.
[16]崔春艳,张红医,吴兴强,等.分散固相萃取-液相色谱-串联质谱法测定谷物、蔬菜、水果中27种新型杀菌剂[J].色谱,2017,5(5):487-494.
[17]孙亚米,吕燕,吴银良.液相色谱-串联质谱法快速测定果蔬中16种新型酰胺类杀菌剂残留量[J].食品科学,2015,17(12):230-236.
[18]周霞,陈万勤,陈晶燕,等.QuEChERS-高效液相色谱-串联质谱法测定春笋中4种农药残留[J].中国食品卫生杂志,2018,30(5):486-490.
[19]孟志娟,黄云霞,赵丽敏,等.气相色谱-串联质谱法测定水果中50种农药残留[J].色谱,2018,36(9):917-924.
[20]李晔,赵丹莹,郭爱华,等.分散固相萃取-气相色谱-三重四级杆串联质谱法测定代用茶中14种农药残留[J].卫生研究,2018,47(4):621-627.
[21]蓝梦哲,林绪,刘雅琼,等.液相色谱-串联质谱法同时测定8种花草茶中77种农药残留[J].色谱,2018,36(9):938-945.
[22]GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].
[2]魏畅,傅红,郑俊超,等.QuECHERS-液质联用同步检测蘑菇中多菌灵等3种杀菌剂残留[J].中国食品学报,2016,6(11):189-195.
[3]张其才,董茂锋,宋卫国,等.超高效液相色谱法检测啶虫脒在工厂化双孢蘑菇栽培中的残留[J].农药学学报,2016,17(3):373-379.
[4]李琴,朱科学,周惠明.固相微萃取-气相色谱-质谱及气相色谱嗅闻技术分析双孢蘑菇汤的风味活性物质[J].食品科学,2011,22(16):300-304.
[5]王雪平,闫凯.固相萃取-气相色谱-质谱法测定饮用水中15种农药残留量[J].理化检验(化学分册),2017,53(4):437-441.
[6]侯雪,韩梅,邱世婷,等.改进的Qu ECh ERS气相色谱-串联质谱法测定草莓中21种杀菌剂残留[J].农药学学报,2017,11(1):46-52.
[7]程寿峰,魏绍峰,王兴宁,等.气相色谱-质谱法测定大米中15种苯氧羧酸类除草剂的残留量[J].理化检验(化学分册),2017,53(11):1281-1285.
[8]李婵君,李柱梅,秦喜玲,等.液相色谱-串联质谱法测定水产品中磺胺类及喹诺酮类药物残留量[J].理化检验(化学分册),2017,23(5):527-531.
[9]Elisa Helena da Costa Morais,Carol Hollingworth Collins,Isabel Cristina Sales Fontes Jardim.Pesticide determination in sweet peppers using Qu ECh ERS and LC-MS/MS[J].Food Chemistry,2018(249):77-83
[10]李继革,王玉飞,施家威,等.固相萃取-气相色谱-串联质谱法测定水果中11种三唑类杀菌剂[J].色谱,2012,6(03):262-266.
[11]Ferreira J A,Ferreira J M S,Talamini V,et al.Determination of pesticides in coconut(Cocos nucifera Linn.)water and pulp using modified Qu ECh ERS and LC-MS/MS[J].Food Chemistry,213(2016):616-624
[12]谢建军,陈捷,李菊,等.改良Qu ECh ERS法结合气相色谱串联质谱测定果蔬中20种杀菌剂[J].食品安全质量检测学报,2013,4(1):82-88.
[13]彭芳,雷美康,徐佳文,等.QuEChERS净化-超高效液相色谱-串联质谱法测定柑橘中7种保鲜剂的残留量[J].理化检验(化学分册),2016,52(9):1007-1010.
[14]Zhan Xiu-ping,Ma Lin,Huang Lan-qi,et al.The optimization and establishment of Qu ECh ERS-UPLC-MS/MSmethod for simultaneously detecting various kinds of pesticides residues in fruits and vegetables[J].Journal of Chromatography B,2017(1060):281-290.
[15]Pastor-Belda M,Garrido I,Campillo N,et al.Combination of solvent ext.ractants for dispersive liquid-liquid micro-extraction of fungicides from water and fruit samples by liquid chromatography with tandem mass spectrometry[J].Food Chemistry,2017(233):69-76.
[16]崔春艳,张红医,吴兴强,等.分散固相萃取-液相色谱-串联质谱法测定谷物、蔬菜、水果中27种新型杀菌剂[J].色谱,2017,5(5):487-494.
[17]孙亚米,吕燕,吴银良.液相色谱-串联质谱法快速测定果蔬中16种新型酰胺类杀菌剂残留量[J].食品科学,2015,17(12):230-236.
[18]周霞,陈万勤,陈晶燕,等.QuEChERS-高效液相色谱-串联质谱法测定春笋中4种农药残留[J].中国食品卫生杂志,2018,30(5):486-490.
[19]孟志娟,黄云霞,赵丽敏,等.气相色谱-串联质谱法测定水果中50种农药残留[J].色谱,2018,36(9):917-924.
[20]李晔,赵丹莹,郭爱华,等.分散固相萃取-气相色谱-三重四级杆串联质谱法测定代用茶中14种农药残留[J].卫生研究,2018,47(4):621-627.
[21]蓝梦哲,林绪,刘雅琼,等.液相色谱-串联质谱法同时测定8种花草茶中77种农药残留[J].色谱,2018,36(9):938-945.
[22]GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].