摘要
建立了同时适用于蜂胶及以其为原料的保健食品中氯霉素残留的检测方法。样品中的蜂胶经乙醇溶解,以4%(质量分数)乙酸铅溶液沉淀具有邻二酚羟基结构的黄酮类成分,在碱性条件下进一步去除不含此结构的黄酮类干扰物,并以甲基叔丁基醚为提取溶剂,有效减少样品中极性干扰物和保健食品辅料(如聚乙二醇、甘油等)的共提取。试样溶液经HPLC-MS/MS测定,内标法定量。线性范围为0. 20～50. 0μg/L,相关系数为0. 999 8;方法检出限为0. 03μg/kg,定量限为0. 1μg/kg;不同基质的回收率为86. 0%～114. 4%,相对标准偏差为0. 3%～4. 9%。该方法通用性强,操作简便,灵敏度高,抗干扰能力强,推广应用前景良好。
A method for determining chloramphenicol(CAP)in both propolis and propolis-derived dietary supplements was developed by utilizing high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).The flavones in the samples were removed with a lead acetate solution and ammonia,and the fat-soluble interferences,such as beewax and vegetable oils,were removed with n-hexane after the sample dissolved in ethanol.Tert-butyl methyl ether was used as the back-extraction solvent to reduce co-extracting compounds,such as polyethylene glycol 400(PEG 400)and glycerol,which are common adjuvants of dietary supplements,and some polar interferences.CAP was detected by HPLC-MS/MS and quantified by the internal standard method.The calibration curve showed a good linearity in the range of 0.20-50.0μg/L.The limits of detection and the limits of quantification were 0.03 and 0.1μg/kg,respectively.The recoveries in four different matrices at three spiked levels were in the 86.0%-114.4%range with the relative standard deviations from 0.3%to 4.9%.With the advantages of excellent universality,ease of operation,high sensitivity,and strong anti-interference capability,the proposed method was suitable for the determination of CAP in both propolis and propolis-derived dietary supplements.
作者
温家欣
吴凤丹
曹雅静
何嘉雯
黄志业
黄艳婷
谭婉清
罗文静
赖宇红
WEN Jiaxin;WU Fengdan;CAO Yajing;HE Jiawen;HUANG Zhiye;HUANG Yanting;TAN Wanqing;LUO Wenjing;LAI Yuhong(Guangdong Institute for Drug Control,Guangzhou 510663,China)
出处
《色谱》
CAS
CSCD
北大核心
2018年第12期1284-1289,共6页
Chinese Journal of Chromatography
基金
广东省省级科技计划项目(2013B090200059)~~
关键词
高效液相色谱-串联质谱
氯霉素
蜂胶
保健食品
软胶囊
硬胶囊
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)
chloramphenicol
propolis
health food
soft capsule
hard capsule
作者简介
通讯联系人.温家欣,Tel:(020)32079725,E-mail:ellawen224@qq.com.
