超高效液相色谱-串联质谱法测定薏仁米中25种磺酰脲类除草剂残留  

Determination of 25 sulfonylurea herbicide residues in coix seed kernels by ultra performance liquid chromatography-tandem mass spectrometry

作　　者：王显贵 吴小毛[1] 杨晓凤[3] 刘炜[3] WANG Xiangui;WU Xiaomao;YANG Xiaofeng;LIU Wei(Guizhou University,Guiyang 550025,Guizhou,China;Agricultural and Rural Bureau of Xingren City,Xingren 562300,Guizhou,China;Analysis and Testing Center of Sichuan Academy of Agricultural Sciences,Chengdu 610066,China)

机构地区：[1]贵州大学,贵州贵阳550025 [2]兴仁市农业农村局,贵州兴仁562300 [3]四川省农业科学院分析测试中心,四川成都610066

出　　处：《世界农药》2021年第5期49-56,共8页World Pesticide

基　　金：国家自然科学基金(221267007);贵州大学培育项目[贵大培育(2019)09号]。

摘　　要：通过改进QuEChERS前处理方法,采用超高效液相色谱-串联质谱法(UPLC-MS/MS)建立了同时测定薏仁米中25种磺酰脲类除草剂残留的分析方法。样品经乙腈(含1%甲酸)提取,QuEChERS方法净化,以Waters ACQUITY UPLC CSH C_(18)Column(2.1 mm×100 mm,1.7μm)进行液相分离,以甲醇-水(含0.1%甲酸及10 mmol/L甲酸铵)为流动相进行梯度洗脱,流速为0.3 mL/min,三重四极杆串联质谱以正离子多重反应监测模式(MRM)进行测定,外标法定量。结果表明,在检测浓度范围内,25种除草剂的质量浓度与对应的峰面积间均呈良好的线性关系,相关系数(r)均大于0.99。在5.0~500μg/kg添加水平下,回收率为85.9%~103.2%,相对标准偏差为1.7%~7.5%,定量限(LOQs)为0.017~1.41μg/kg,基质效应为0.83~1.13。该方法前处理简单,分析时间短,准确度和灵敏度高,适合于薏仁米样品中25种磺酰脲类除草剂残留实际检测需要。A method for simultaneous determination of 25 sulfonylurea herbicide residues in coix seeds was developed by improving the pretreatment method of QuEChERS and using ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The samples were extracted with acetonitrile,cleaned up by developed QuEChERS method.The separation was performed on a waters ACQUITY UPLC CSH C18 Column(2.1 mm×100 mm,1.7μm),the mixture of methanol,0.1%formic acid and 10 mmol/L ammonium aqueous solution was used as mobile phase in gradient elution,and the flow rate was 0.3 mL/min.Targeted compounds were analyzed using UPLC-MS/MS in multiple reaction monitoring(MRM)mode via positive electrospray ionization(ESI^(+)),and quantified by external standard method.Results showed that there were good linear relationships between the concentrations and their responding values of 25 herbicides under the detection concentration,with correlation coefficients higher than 0.99.The recoveries of the target compounds in two matrices were both 85.9%-103.2%,and the RSDs were both 1.7%-7.5%.the limits of quantitation(LOQs)were 0.017-1.41μg/kg,the matrix effects were 0.83-1.13.This method is simple,rapid,time-saving,high sensitive and accuracy,and suitable for the actual detection of 25 sulfonylurea herbicide residues in coix seed samples.

关 键 词：超高效液相色谱-串联质谱 薏仁米 磺酰脲类除草剂 残留 

分 类 号：TQ450.2[化学工程—农药化工]