改进QuEChERS/超高效液相色谱-串联三重四极杆质谱法快速检测茶叶中百草枯和敌草快残留  

Rapid Determination of Paraquat and Diquat Residues in Tea by QuEChERS/Ultra-High Performance Liquid Chromatography-Tandem Quadrupole Mass Spectrometry

作　　者：唐燕花 高英楠 陈江艳 郭心怡 李绍涌 李悦 周振[1] 高伟[1,3,4] TANG Yan-Hua;GAO Ying-Nan;CHEN Jiang-Yan;GUO Xin-Yi;LI Shao-Yong;LI Yue;ZHOU Zhen;GAO Wei(Institute of Mass Spectrometry and Atmospheric Environment,College of Environment and Climate,Jinan University,Guangzhou 510632,China;Guangzhou Hexin Instrument Co.Ltd.,Guangzhou 510632,China;Key Laboratory of Testing and Quality Control for Petroleum Products,State Administration for Market Regulation,Shenyang 110144,China;Guangdong Provincial Engineering Research Center for On-line Source Apportionment System of Air Pollution,Guangzhou 510632,China)

机构地区：[1]暨南大学环境与气候学院,质谱仪器与大气环境研究所,广州510632 [2]广州禾信仪器股份有限公司,广州510632 [3]国家市场监督管理总局重点实验室(石油产品检测与质量控制),沈阳110144 [4]广东省大气污染在线源解析系统工程研究中心,广州510632

出　　处：《分析化学》2024年第10期1619-1627,共9页Chinese Journal of Analytical Chemistry

摘　　要：通过改进QuEChERS前处理方法,结合超高效液相色谱-串联三重四极杆质谱技术,建立了一种快速检测茶叶中百草枯和敌草快的方法。4种茶叶粉末经乙腈-0.1%甲酸溶液(3∶7,V/V)超声提取后,以400 mg C18和400 mg PSA作为净化剂对上清液进行净化,采用亲水型HILIC色谱柱(100 mm×2.1 mm,1.8μm)进行分离,0.1%甲酸-水(含5 mmol/L甲酸铵)和乙腈为流动相进行等度洗脱,在电喷雾电离源(ESI+)下,采用多反应监测扫描方式(MRM)进行测定,通过基质匹配标准溶液外标法进行定量分析。结果表明,在4种茶叶基质中,百草枯含量在0.18~200μg/kg范围内、敌草快含量在0.36~200μg/kg范围内线性关系均良好,相关系数(R2)分别在0.9939~0.9976和0.9959~0.9987范围内,方法检出限分别为0.06和0.12μg/kg,定量限分别为0.18和0.36μg/kg,茶叶样品的平均加标回收率为84.4%~128.8%,相对标准偏差(RSD)为0.6%~13.5%。本方法操作简单高效、定量分析准确、检出限低,可用于对茶叶样品中百草枯和敌草快的快速检测。A rapid analytical method for determination of paraquat and diquat in tea samples was established by improving the QuEChERS pre-treatment method combined with ultra-high performance liquid chromatographytandem quadrupole mass spectrometry(UPLC-MS/MS).Four kinds of tea powder were extracted by using acetonitrile-0.1%formic acid solution(3∶7,V/V)and ultrasonic treatment,and the supernatant was purified with 400 mg C18 and 400 mg PSA and separated on hydrophilic HILIC(100 mm×2.1 mm,1.8μm)column by using 0.1%formic acid aqueous solution(Containing 5 mmol/L ammonium formate)and acetonitrile as mobile phases.In the electrospray ion source positive ion mode(ESI+),multiple reaction monitoring scanning technology(MRM)was used for determination,and the matrix-matched standard solution external standard method was used for quantitative analysis.The results showed that paraquat obtained good linear relationship in the content range of 0.18–200μg/kg and diquat obtained good linear relationship in the content range of 0.36–200μg/kg,and the correlation coefficients(R2)were 0.9939–0.9976 and 0.9959–0.9987,respectively.The limits of detection(LODs)were 0.06 and 0.12μg/kg,and the limits of quantitation(LOQs)were 0.18 and 0.36μg/kg,respectively.The average spiked recoveries for tea samples varied from 84.4%to 128.8%,with the relative standard deviations(RSDs)from 0.6%to 13.5%.The method was simple and efficient,with accurate quantification ability and low detection limit,which could realize efficient determination of paraquat and diquat in tea samples.

关 键 词：QUECHERS 超高效液相色谱-串联三重四极杆质谱法 茶叶 百草枯 敌草快 

分 类 号：O657.63[理学—分析化学] TS272.7[理学—化学]