QuEChERS结合高效液相色谱串联质谱法同时测定马铃薯中的噻虫嗪、氟啶虫酰胺及其代谢物
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摘要
[目的]建立高效液相色谱串联质谱法检测马铃薯中噻虫嗪及其代谢物(噻虫胺)、氟啶虫酰胺及其代谢物(TFNA和TFNG)的方法。[方法]样品经含1%乙酸的乙腈提取,QuEChERS法净化,反相C_(18)色谱柱分离,以0.1%乙酸水-甲醇为流动相进行梯度洗脱,流速为0.3 mL/min,用高效液相色谱串联质谱分析,采用多反应离子检测模式(MRM)检测,外标法定量。[结果]在0.001～0.2 mg/L范围内5种农药线性良好(r≥0.9984),在0.05～1.0 mg/kg添加水平下,5种农药平均添加回收率均在73.7%～106.3%之间,相对标准偏差(RSD)在0.8%～16.5%之间,方法定量限(LOQ)为0.05 mg/kg。[结论]该方法快速简便,能满足马铃薯中噻虫嗪、氟啶虫酰胺及其代谢物的快速检测要求。
[Aims]A new method was developed for residual analysis of thiamethoxam and its metabolites clothianidin,flonicamid and its two metabolites such as TFNA and TFNG in potato by high performance liquid chromatographytandem mass spectrometry. [Methods]Thiamethoxam and its metabolites clothianidin, flonicamid and its two metabolites such as TFNA and TFNG residues in potato were extracted with acetonitrile containing 1% acetic acid and purified by QuEChERS method. Then reversed-phase C_(18) chromatographic column was used to separate the residues,the mixture of 0.1% acetic acid aqueous solution and methanol was used as mobile phase in gradient elution with the flow rate of 0.3 mL/min. Finally, the residues were detected by HPLC-MS/MS under multiple reaction monitoring mode(MRM) and quantified by external standard method. [Results]The results showed that good linearities for the five analytes were observed in the concentration range of 0.001-0.2 mg/L with the correlation coefficients(r) not less than0.9984. The limits of quantification(LOQs) were 0.05 mg/kg. The average recoveries at the fortified levels of 0.05, 0.2 and 1.0 mg/kg were in the range of 73.7-106.3% with the relative standard deviations of 0.8-16.5%. [Conclusions]With the advantages of rapidness, simplicity, high sensitivity and good reproducibility, the method is suitable for the determination of thiamethoxam, flonicamid and their metabolites residues in potato.
[Aims]A new method was developed for residual analysis of thiamethoxam and its metabolites clothianidin,flonicamid and its two metabolites such as TFNA and TFNG in potato by high performance liquid chromatographytandem mass spectrometry. [Methods]Thiamethoxam and its metabolites clothianidin, flonicamid and its two metabolites such as TFNA and TFNG residues in potato were extracted with acetonitrile containing 1% acetic acid and purified by QuEChERS method. Then reversed-phase C_(18) chromatographic column was used to separate the residues,the mixture of 0.1% acetic acid aqueous solution and methanol was used as mobile phase in gradient elution with the flow rate of 0.3 mL/min. Finally, the residues were detected by HPLC-MS/MS under multiple reaction monitoring mode(MRM) and quantified by external standard method. [Results]The results showed that good linearities for the five analytes were observed in the concentration range of 0.001-0.2 mg/L with the correlation coefficients(r) not less than0.9984. The limits of quantification(LOQs) were 0.05 mg/kg. The average recoveries at the fortified levels of 0.05, 0.2 and 1.0 mg/kg were in the range of 73.7-106.3% with the relative standard deviations of 0.8-16.5%. [Conclusions]With the advantages of rapidness, simplicity, high sensitivity and good reproducibility, the method is suitable for the determination of thiamethoxam, flonicamid and their metabolites residues in potato.
引文
[1]徐爱霞,魏钊.新型烟碱类杀虫剂——隆施[J].西北园艺(果树),2015(2):38.
[2]SUGANTHI A,NIKITA S A,KOUSIKA J,et al.Determination of Thiamethoxam Residues in Banana Stem and Fruit Through LC-MS/MS[J].Environmental Monitoring&Assessment,2018,190(5):293.
[3]陈国峰,李雪茹,刘峰,等.高效氯氟氰菊酯、噻虫嗪及其代谢物噻虫胺在小麦中的残留及消解动态分析[J].麦类作物学报,2018,38(1):119-125.
[4]LPEZRUIZ R,ROMEROGONZ LEZ R,MARTíNEZ VIDALJ L,et al.Determination of Flonicamid and Its Metabolites in Bell Pepper Using Ultra High Performance Liquid Chromatography Coupled to High Resolution Massspectrometry(Orbitrap)[J].Food Additives&Contaminants,2016,33(11):1685-1692.
[5]The Japan Food Chemical Research Foundation,(2012).Table of MRLs for Agricultural Chemicals[EB/OL].Http://www.m5.ws001.squarestart.ne.jp/foundation/agrdtl.php?a_inq=65450.
[6]EU Pesticides Database.Pesticide EU-MRLs.Regulaton(EC)No 396/2005[EB/OL].Http://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/public/?event=pesticide.residue.selection&language=EN.
[7]GB 2763-2016.食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[8]KO A Y,EL-ATY A M A,RAHMAN M M,et al.A Modified QuEChERS Method for Simultaneous Determination of Flonicamid and Its Metabolites in Paprika Using Tandem Mass Spectrometry[J].Food Chemistry,2014,157(4):413-420.
[9]蒋梦云,巩文雯,刘庆菊,等.噻虫嗪及其代谢产物在盆栽辣椒和土壤中的残留动态和膳食风险评估[J].农药,2018,57(9):662-665.
[10]王博,侯志广,方楠,等.噻虫嗪及其代谢物在大葱中的消解动态及最终残留[J].农药,2018,57(9):671-674.
[11]刘艳萍,王思威,孙海滨,等.噻虫嗪及其代谢物噻虫胺在节瓜中的消解动态及初步膳食风险评估[J].农药学学报,2018,20(2):211-216.
[12]鞠光秀,孙克,张敏恒.氟啶虫酰胺分析方法述评[J].农药,2013,52(8):620-623.
[13]陈国,孙亚米,杨挺,等.液相色谱-串联质谱法测定黄瓜和苹果中氟啶虫酰胺及其代谢产物残留量[J].色谱,2012,30(6):555-559.
[14]刘炎,欧阳迪庆,叶玉凤,等.QuEChERS结合超高效液相色谱-串联质谱法同时测定番茄中噻虫嗪、噻虫胺、螺虫乙酯及其代谢物残留[J].分析测试学报,2017,36(12):1431-1438.
[15]刘亚娟,侯志广,梁爽,等.70%扑草净·乙草胺SE在花生中的残留分析方法[J].农药,2017,56(3):193-196.
[2]SUGANTHI A,NIKITA S A,KOUSIKA J,et al.Determination of Thiamethoxam Residues in Banana Stem and Fruit Through LC-MS/MS[J].Environmental Monitoring&Assessment,2018,190(5):293.
[3]陈国峰,李雪茹,刘峰,等.高效氯氟氰菊酯、噻虫嗪及其代谢物噻虫胺在小麦中的残留及消解动态分析[J].麦类作物学报,2018,38(1):119-125.
[4]LPEZRUIZ R,ROMEROGONZ LEZ R,MARTíNEZ VIDALJ L,et al.Determination of Flonicamid and Its Metabolites in Bell Pepper Using Ultra High Performance Liquid Chromatography Coupled to High Resolution Massspectrometry(Orbitrap)[J].Food Additives&Contaminants,2016,33(11):1685-1692.
[5]The Japan Food Chemical Research Foundation,(2012).Table of MRLs for Agricultural Chemicals[EB/OL].Http://www.m5.ws001.squarestart.ne.jp/foundation/agrdtl.php?a_inq=65450.
[6]EU Pesticides Database.Pesticide EU-MRLs.Regulaton(EC)No 396/2005[EB/OL].Http://ec.europa.eu/food/plant/pesticides/eu-pesticides-database/public/?event=pesticide.residue.selection&language=EN.
[7]GB 2763-2016.食品安全国家标准食品中农药最大残留限量[S].北京:中国标准出版社,2016.
[8]KO A Y,EL-ATY A M A,RAHMAN M M,et al.A Modified QuEChERS Method for Simultaneous Determination of Flonicamid and Its Metabolites in Paprika Using Tandem Mass Spectrometry[J].Food Chemistry,2014,157(4):413-420.
[9]蒋梦云,巩文雯,刘庆菊,等.噻虫嗪及其代谢产物在盆栽辣椒和土壤中的残留动态和膳食风险评估[J].农药,2018,57(9):662-665.
[10]王博,侯志广,方楠,等.噻虫嗪及其代谢物在大葱中的消解动态及最终残留[J].农药,2018,57(9):671-674.
[11]刘艳萍,王思威,孙海滨,等.噻虫嗪及其代谢物噻虫胺在节瓜中的消解动态及初步膳食风险评估[J].农药学学报,2018,20(2):211-216.
[12]鞠光秀,孙克,张敏恒.氟啶虫酰胺分析方法述评[J].农药,2013,52(8):620-623.
[13]陈国,孙亚米,杨挺,等.液相色谱-串联质谱法测定黄瓜和苹果中氟啶虫酰胺及其代谢产物残留量[J].色谱,2012,30(6):555-559.
[14]刘炎,欧阳迪庆,叶玉凤,等.QuEChERS结合超高效液相色谱-串联质谱法同时测定番茄中噻虫嗪、噻虫胺、螺虫乙酯及其代谢物残留[J].分析测试学报,2017,36(12):1431-1438.
[15]刘亚娟,侯志广,梁爽,等.70%扑草净·乙草胺SE在花生中的残留分析方法[J].农药,2017,56(3):193-196.