粮谷中杀螺胺乙醇胺盐残留量的测定
Method for Determination of Niclosamide-Olamine Residues in Grains
郭雨 1施亚申 2严静华 1林桦3
作者信息
- 1. 江苏安舜技术服务有限公司 苏州 215332
- 2. 苏州海关综合技术中心 苏州 215104
- 3. 早康枸杞股份有限公司 中卫 755100
- 折叠
摘要
本研究建立了一种液相色谱-串联质谱法测定粮谷中杀螺胺乙醇胺盐残留量的方法.采用改进的QuEChERS方法,样品经一定体积比的氨水乙腈超声提取,冷冻高速离心,N-丙基乙二胺(PSA)分散萃取净化材料净化,采用安捷伦Zorbax C18 色谱柱分离,高效液相色谱串联质谱仪检测,通过外标法准确定量.杀螺胺乙醇胺盐在0.2～20.0 μg/L浓度范围内,7个空白基质标准曲线浓度点具有较好的线性关系,相关系数R2＞0.995,杀螺胺乙醇胺盐的检出限为0.3 μg/kg,定量限为1.0 μg/kg;在1.0 μg/kg、5.0 μg/kg和10.0 μg/kg 3个不同浓度加标水平下,粮谷中杀螺胺乙醇胺盐6次平行试验结果的平均回收率为83.5%～122.7%,相对标准偏差在1.1%～9.4%之间.结果表明,该方法样品前处理操作简便、耗时短、检测耗材成本低、结果重复性佳,能够满足日常粮谷中杀螺胺乙醇胺盐残留的检测要求.
Abstract
A method was established to determine residue of niclosamide-olamine in grains by LC-MS/MS.Using the improved QuEChERS method,the samples were ultrasonically extracted by a certain volume ratio of ammonia acetonitrile,centrifuged at high speed in a refrigerated state,purified with PSA.They were separated by Agilent Zorbax C18 chromatographic column,detected by high-performance liquid chromatography tandem mass spectrometer,and accurately quantified by external standard method.In the concentration range of 0.2-20.0 μg/L,the concentration points of the 7 blank matrix standard curves had a good linear relationship,with the correlation coefficient(R²)＞0.995,and the detection limit of niclosamide-olamine was 0.3 μg/kg and the limit of quantification was 1.0 μg/kg.The average recoveries of six parallel tests of niclosamide-olamine in grains were 83.5%-122.7%,and the relative standard deviations were 1.1%-9.4%under three different concentration spike levels of 1.0 μg/kg,5.0 μg/kg and 10.0 μg/kg.This method has simple sample pre-treatment,short analysis time,low cost of detection consumables,and good reproducibility.It can meet the detection requirements for the residues of niclosamide-olamine in grains.
关键词
粮谷/杀螺胺乙醇胺盐/QuEChERSKey words
grain/niclosamide-olamine/QuEChERS引用本文复制引用
出版年
2024
NETL
NSTL
万方数据