天津农业科学2024,Vol.30Issue(8) :59-66.DOI:10.3969/j.issn.1006-6500.2024.08.009

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

绳慧珊 李娜 刘磊 牛艺融 郭永泽 张玉婷
天津农业科学2024,Vol.30Issue(8) :59-66.DOI:10.3969/j.issn.1006-6500.2024.08.009

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

绳慧珊 1李娜 2刘磊 2牛艺融 2郭永泽 2张玉婷1
扫码查看

作者信息

  • 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;天津海世达检测技术有限公司,天津 300381
  • 2. 天津市农业科学院 农产品质量安全与营养研究所,天津 300381
  • 折叠

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.

Abstract

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-cal-cium 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 0.196 14 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

Key words

sweet potato/prohexadione-calcium/residue/ultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)/assay

引用本文复制引用

基金项目

天津市蔬菜现代农业技术体系创新团队(ITTVRS2024019)

&&(23YFZCSN00200)

出版年

2024
天津农业科学
天津农业科学院信息研究所

天津农业科学

影响因子:0.705
ISSN:1006-6500
段落导航相关论文