首页|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

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

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

sweet potatoprohexadione-calciumresidueultra high performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)assay

绳慧珊、李娜、刘磊、牛艺融、郭永泽、张玉婷

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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

甘薯 调环酸钙 残留 超高效液相色谱-串联质谱 含量测定

天津市蔬菜现代农业技术体系创新团队&&

ITTVRS202401923YFZCSN00200

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
年,卷(期):2024.30(8)