亲水作用色谱-串联质谱法测定蔬菜中草甘膦及其代谢物残留  

Determination of Glyphosate and Its Metabolite Residues in Vegetables by Hydrophilic Interaction Chromatography Tandem Mass Spectrometry

作　　者：孟繁磊[1] 谭莉 范宏 张惠峰 张慧[1] 樊慧梅[1] MENG Fanlei;TAN Li;FAN Hong;ZHANG Huifeng;ZHANG Hui;FAN Huimei(Institute of Agricultural Quality Standard and Testing Testing Technology,Jilin Academy of Agricultural Sciences,Agricultural Product Quality and Safety Risk Assessment Laboratory of the Ministry of Agriculture and Rural Areas(Changchun),Jilin Key Laboratory of Agricultural Environment and Agricultural Product Safety,Changchun 130033,China)

机构地区：[1]吉林省农业科学院,农业质量标准与检测技术研究所,农业农村部农产品质量安全风险评估实验室(长春),吉林省农业环境与农产品安全重点实验室,吉林长春130033

出　　处：《食品科技》2022年第9期271-276,共6页Food Science and Technology

基　　金：吉林省农业科学院农业质量标准与检测技术研究所发展基金项目(ZBS20Q03)。

摘　　要：建立了基于亲水作用色谱串联质谱法测定蔬菜中草甘膦(GLY)及其代谢产物氨甲基膦酸(AMPA)的方法。蔬菜样品匀浆后经含1%甲酸的甲醇水溶液(v:v=1:1)涡旋、超声波提取,用Oasis PRiME HLB固相萃取小柱净化后,以5 mmol/L乙酸铵水溶液(pH11)和乙腈溶液作为流动相在Dikma Polyamino HILIC色谱柱上进行梯度洗脱与分离,在电喷雾负离子模式下进行反应监测(MRM),同位素内标法定量分析。优化了液相色谱与质谱的仪器条件和样品前处理条件对草甘膦及其代谢产物氨甲基膦酸测定的影响。实验结果表明,草甘膦及其代谢产物氨甲基膦酸在2~200μg/L呈现良好的线性关系(线性相关系数R2>0.999),检出限和定量限分别为0.002 mg/kg和0.005 mg/kg;在0.005、0.01、0.05 mg/kg 3个添加水平下,加标回收率范围为88.2%~103.1%,相对标准偏(RSD)为0.9%~7.6%。该方法与现行标准SN/T 1923—2007进行比对,结果表明,2种方法检测结果无显著性差异,证明该方法准确可靠,实际可行。但是该方法前处理简便快速,准确性好、灵敏度高、检测时间短、成本低,更适合蔬菜中草甘膦及其代谢物残留量的日常监测。A method for the determination of glyphosate(Gly)and its metabolite aminomethylphosphonic acid(AMPA)in vegetables by hydrophilic interaction chromatography tandem mass spectrometry was established.Vegetable samples were homogenized and then extracted with methanol solution of 1%formic acid(v:v=1:1)and extracted by ultrasonic wave.After purification with Oasis PRiME HLB solid phase extraction column,5 mmol/L aqueous solution(pH11)and acetonitrile solution were used as mobile phase to carry out step elution and separation on Dikma poiyamino HILIC column,and the reaction was monitored under electrospray ionization mode(MRM).Quantitative analysis of matrix matching isotope internal standard method.The effects of instrument conditions of liquid chromatography and mass spectrometry and sample pretreatment conditions on the determination of glyphosate and its metabolite aminomethylphosphonic acid were optimized.The results showed that glyphosate and its metabolite aminomethylphosphonic acid were in the range of 2~200μg/L.(linear correlation coefficient R2>0.999),and the detection limit and quantitative limit were 0.002 and 0.005 mg/kg respectively;At the addition levels of 0.005 mg/kg,0.01 mg/kg and 0.05 mg/kg,the recovery ranged from 88.2%to 103.1%,and the relative standard deviation(RSD)ranged from 0.9%to 7.6%.This method is compared with the current standard SN/T 1923—2007.The results show that there is no significant difference between the two methods,which proves that this method is accurate,reliable and practical.However,this method has the advantages of simple and rapid pretreatment,good accuracy,high sensitivity,short detection time and low detection cost.It is more suitable for the daily monitoring of glyphosate and its metabolite residues in vegetables.

关 键 词：亲水作用色谱 蔬菜 草甘膦 氨甲基膦酸 内标法 

分 类 号：TS207.53[轻工技术与工程—食品科学] O[轻工技术与工程—食品科学与工程]