Experimental Techniques and MethodsDetermination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Propolis and Propolis-derived Dietary Supplements by High Performance Liquid Chromatography-Tandem Mass Spectrometry
|更新时间:2023-04-18
|
Experimental Techniques and MethodsDetermination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Propolis and Propolis-derived Dietary Supplements by High Performance Liquid Chromatography-Tandem Mass Spectrometry
Vol. 39, Issue 7, Pages: 887-893(2020)
作者机构:
1. 东盟食品检验检测中心,广西
2. 广西中医药大学药学院
作者简介:
基金信息:
DOI:
CLC:
扫 描 看 全 文
Experimental Techniques and MethodsDetermination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Propolis and Propolis-derived Dietary Supplements by High Performance Liquid Chromatography-Tandem Mass Spectrometry. [J]. 39(7):887-893(2020)
DOI:
Experimental Techniques and MethodsDetermination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Propolis and Propolis-derived Dietary Supplements by High Performance Liquid Chromatography-Tandem Mass Spectrometry. [J]. 39(7):887-893(2020)DOI:
Experimental Techniques and MethodsDetermination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Propolis and Propolis-derived Dietary Supplements by High Performance Liquid Chromatography-Tandem Mass Spectrometry
A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS) was established for the determination of chloramphenicol,thiamphenicol and florfenicol in propolis and propolis derived dietary supplements including tablet,hard capsule and soft capsule.The samples were dissolved and dispersed with 0.1 mol/L hydrochloric acid solution,blended well with a vortex mixer,followed by ultrasonical extraction and purification with an HLB solid phase extraction column(SPE) tandemly connected with a NH2-SPE column.The extract was separated on an Waters ACQUITY UPLC-BEH C18 column(2.1 mm×100 mm,1.7 μm) by gradient elution using a mobile phase consisting of 0.1% formic acid and acetonitrile.The analytes were analyzed by HPLC-MS/MS with electrospray ionization(ESI) source in negative ion mode,and quantified by external standard method.Under the optimal conditions,there were good linear relationships for 3 analytes in the concentration range of 0.10-20.0 μg/L with correlation coefficients(r2) larger than 0.999.The limits of detection(LOD) and limits of quantitation(LOQ) for three targets in propolis,propolis tablet and propolis soft capsule were in the ranges of 0.037-0.083 μg/kg and 0.12-0.28 μg/kg,while the LODs and LOQs for those in propolis hard capsule were 0.39-0.47 μg/kg and 1.28-1.57 μg/kg,respectively.The recoveries at spiked levels of 2.5,5.0,10.0 μg/kg were between 66.6% and 120%,with relative standard deviations(RSD) of 0.80%-11%.This method was applied to the detection on 45 actual samples collected in laboratory.The samples of propolis derived dietary supplements were detected positive for chloramphenicol and florfenicol,among which the positive detection rate for chloramphenicol was 22.22%,and the maximum residue was 14.32 μg/kg,while the positive detection rate for florfenicol was 17.78%,and the maximum residue was 21.62 μg/kg.With the characteristics of simplicity,high sensitivity and good reproducibility,the method could meet the requirements for determination of chloramphenicol,thiamphenicol and florfenicol residues in propolis and propolis-derived dietary supplements.
关键词
高效液相色谱-串联质谱(HPLC-MS/MS)蜂胶蜂胶原料保健食品氯霉素甲砜霉素氟甲砜霉素
Keywords
high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)propolispropolis derived dietary supplementschloramphenicolthiamphenicolflorfenicol
Simultaneous Determination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Feedstuff by Isotope Dillution High Performance Liquid Chromatography-Tandem Mass Spectrometry
Simultaneous Determination of Chloramphenicol,Thiamphenicol and Florfenicol Residues in Feed by High Performance Liquid Chromatography-Tandem Mass Spectrometry
The Strategy of Multi-wavelength Automatic Fusion Fingerprint and Its Application in Propolis Quality Evaluation
Aptamer Electrochemiluminescence Sensor for Sensitive Detection of Chloramphenicol
Related Author
No data
Related Institution
湛江出入境检验检疫局检验检疫技术中心
江苏出入境检验检疫局动植物与食品检测中心
淮安出入境检验检疫局
Center for Food Evaluation,State Administration for Market Regulation
Zhejiang Traditional Chinese Medicine Research Institute Co.,Ltd.