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QuEChERS-液相色谱-串联质谱法测定蜂产品中克百威和3-羟基克百威的残留量
          
Determination of Residues of Carbofuran and 3-Hydroxycarbofuran in Bee Products by Liquid Chromatography Tandem Mass Spectrometry with QuEChERS

摘    要
提出了QuEChERS前处理结合液相色谱-串联质谱法(LC-MS/MS)测定蜂产品(蜂蜜,蜂胶和蜂王浆)中克百威及3-羟基克百威的残留量。蜂产品样品使用乙腈提取,用无水硫酸镁脱水,再用无水硫酸镁、乙二胺-N-丙基硅烷化硅胶(PSA)和十八烷基硅烷键合硅胶(C18)混合剂净化,采用Accucore aQ C18色谱柱(150 mm×2.1 mm,2.6 μm)进行分离,以不同体积比的甲醇和含5 mmol·L-1甲酸铵的0.1%(体积分数)甲酸溶液混合液为流动相进行梯度洗脱,多反应监测(MRM)模式下进行质谱检测,外标法定量。结果表明,克百威及3-羟基克百威的质量浓度在0.002~0.100 mg·L-1内与对应的峰面积呈线性关系,克百威和3-羟基克百威在蜂蜜、蜂王浆中的测定下限(10S/N)均为0.01 mg·kg-1,在蜂胶中的测定下限(10S/N)为0.05 mg·kg-1。按照标准加入法进行回收试验,回收率为84.5%~108%,测定值的相对标准偏差(n=6)小于7.0%。
标    签 QuEChERS   液相色谱-串联质谱法   蜂产品   克百威和3-羟基克百威   残留   QuEChERS   liquid chromatography tandem mass spectrometry   bee product   carbofuran and 3-hydroxycarbofuran   residue  
 
Abstract
A method for determination of residues of carbofuran and 3-hydroxycarbofuran in bee products (honey, propolis and royal jelly) was proposed by QuEChERS pretreatment combined with liquid chromatography tandem mass spectrometry (LC-MS/MS). The bee product sample was extracted with acetonitrile, dehydrated by anhydrous magnesium sulfate, and purified with the mixed agent of anhydrous magnesium sulfate, PSA and C18. Accucore aQ C18 column (150 mm×2.1 mm, 2.6 μm) was used for the separation, and the mixtures of methanol and 0.1% (volume fraction) formic acid solution containing 5 mmol·L-1 ammonium formate at different volume ratios were used as the mobile phase for gradient elution. Multiple reaction monitoring (MRM) mode was adopted in MS detection, with external standard method for quantification. As shown by the results, linear relationships between values of the corresponding peak area and mass concentration of carbofuran and 3-hydroxycarbofuran were found in the range of 0.002-0.100 mg·L-1, with lower limits of determination (10S/N) of carbofuran and 3-hydroxycarbofuran in honey and royal jelly of 0.01 mg·kg-1, and those in propolis of 0.05 mg·kg-1. Test for recovery was made by the standard addition method, giving the results in the range of 84.5%-108%, with RSDs (n=6) of the determined values less than 7.0%.

中图分类号 O657.63   DOI 10.11973/lhjy-hx202312004

 
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所属栏目 工作简报

基金项目 国家重点研发计划项目(2019YFC1605403)

收稿日期 2022/11/16

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备注黎天勇,工程师,主要从事食品质量安全检测研究工作

引用该论文: LI Tianyong,LI Ju,WU Shuyue,XI Jing,WANG Lan. Determination of Residues of Carbofuran and 3-Hydroxycarbofuran in Bee Products by Liquid Chromatography Tandem Mass Spectrometry with QuEChERS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2023, 59(12): 1388~1394
黎天勇,李菊,吴舒悦,席静,王岚. QuEChERS-液相色谱-串联质谱法测定蜂产品中克百威和3-羟基克百威的残留量[J]. 理化检验-化学分册, 2023, 59(12): 1388~1394


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