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(C_(18))混合剂净化,采用Accucore aQ C_(18)色谱柱(150 mm×2.1 mm, 2.6μm)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%。
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 Cis.Accucore aQ C_(18)column(150 mm×2.1 mm,2.6μm)was used for the separation,and the mixtures of methanol and o.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 o.01 mg·kg^(-1),and those in propolis of o.05 mg kg^(-1),Test for recovery was made by the standard addition method,giving the results in the range of 84.5%^(-1)08%,with RSDs(n=6)of the determined values less than 7.0%.
作者
黎天勇
李菊
吴舒悦
席静
王岚
LI Tianyong;LI Ju;WU Shuyue;XI Jing;WANG Lan(Technology Center of Guangzhou Customs,Guangzhou 510623,China)
出处
《理化检验（化学分册）》
CSCD
北大核心
2023年第12期1388-1394,共7页
Physical Testing and Chemical Analysis(Part B:Chemical Analysis)
基金
国家重点研发计划项目(2019YFC1605403)。
