甘薯中调环酸钙残留量的超高效液相色谱-串联质谱检测方法  

Residues Determination of Prohexadione-calcium in Sweet Potato by UPLC-MS/MS

作　　者：绳慧珊 李娜[1] 刘磊[1] 牛艺融 郭永泽[1] 张玉婷[1,2] SHENG Huishan;LI Na;LIU Lei;NIU Yirong;GUO Yongze;ZHANG Yuting(Institute of Agro-product Safety and Nutrition,Tianjin Academy of Agricultural Sciences,Tianjin 300381,China;Tianjin High-standard Quality Testing Lab.,Tianjin 300381,China)

机构地区：[1]天津市农业科学院农产品质量安全与营养研究所,天津300381 [2]天津海世达检测技术有限公司,天津300381

出　　处：《天津农业科学》2024年第8期59-66,共8页Tianjin Agricultural Sciences

基　　金：天津市蔬菜现代农业技术体系创新团队(ITTVRS2024019);基于光纤SERS探针的便携式农药残留检测仪关键技术研究(23YFZCSN00200)。

摘　　要：为建立甘薯中调环酸钙残留量的超高效液相色谱-串联质谱检测方法,采用QuEChERS前处理方法,用0.5%甲酸乙腈溶液提取甘薯样品,经氯化钠盐析分层后,取上层有机相浓缩至干,最后用乙腈-0.1%甲酸水(1∶1,V/V)溶液复容后上机检测。结果表明,调环酸钙的最小检出量为1×10-11 g,定量限为0.01 mg·kg^(-1),平均回收率范围为89%~91%,相对标准偏差范围为1%~3%,调环酸钙在0.005~0.500 mg·L^(-1)浓度范围内线性关系良好,相关系数大于0.99,基质效应可忽略不计。在陕西和天津等8个地点进行田间试验,甘薯样品中调环酸钙的残留量均小于0.01 mg·kg^(-1),通过膳食风险评估,调环酸钙的国家估算每日摄入量(NEDI)为0.19614 mg。综上所述,该方法能够方便快捷地检测出调环酸钙在甘薯中的残留量,准确度和精密度均能满足要求,按照推荐剂量和方法施用12%S-诱抗素·调环酸钙可溶粉剂,安全性良好,符合我国相关残留限量的标准。In order to establish a method of UPLC-MS/MS to detect the amount of prohexadione-calcium in sweet potato,using the QuEChERS pre-processing method,sweet potato samples were extracted by 0.5%formic acid-acetonitrile solution,after stratification by sodium chloride salting out,and take the upper organic phase and condense to dry.Finally,it was redissolved by acetonitrile-0.1%formic acid water(1∶1,V/V)solution and tested by machine.The results showed that minimum detection amount of prohexadione-calcium was 1×10-11 g,with the limit of quantification of 0.01 mg·kg^(-1),average recovery of 89%-91%,relative standard deviation of 1%-3%,good linear relationship in the range of 0.005-0.500 mg·L^(-1),with correlation coefficients greater than 0.99,and matrix effects could be negligible.Field trial were conducted at Shanxi and Tianjin and other 8 places,the residues of prohexadione-calcium in sweet potatoe samples were all less than 0.01 mg·kg^(-1).Through dietary risk assessment,the estimated national daily intake(NEDI)of prohexadione-calcium in the general population was 0.19614 mg.To sum up,the method can be used to detect the residual amount of prohexadione-calcium in sweet potato simply and quickly,and the accuracy and precision can meet the requirements,12%trans-abscisic acid·prohexadione-calcium soluble powder is applied in accordance with the recommended dosage and method,with good safety,in line with the relevant residue limit standards of our country.

关 键 词：甘薯 调环酸钙 残留 超高效液相色谱-串联质谱 含量测定 

分 类 号：O657.63[理学—分析化学] S481.8[理学—化学]