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高效液相色谱-串联质谱法同时测定蜂胶、蜂胶原料保健食品中的氯霉素、甲砜霉素与氟甲砜霉素
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杨黎,刘星,廖夏云,刘常凯,余仁连,苏小婷 1.广西-东盟食品检验检测中心2.广西中医药大学药学院 
基金项目:广西食品药品监督管理局科技项目(YJJ16001);广西中医药大学“岐黄工程”高层次人才团队培育项目(2018002);广西高等学校高水平创新团队自主计划(桂教2019-52)
中文摘要:建立了同时测定蜂胶、蜂胶原料保健食品(片剂、硬胶囊、软胶囊3种剂型)中氯霉素、甲砜霉素和氟甲砜霉素残留的高效液相色谱-串联质谱(HPLC-MS/MS)方法。样品经0.1 mol/L盐酸溶解,涡旋混匀,超声提取后,通过HLB柱串接NH2固相萃取柱净化。采用Waters ACQUITY UPLC-BEH C18(2.1 mm×100 mm,1.7 μm)色谱柱进行分离,以0.1%甲酸水-乙腈为流动相梯度洗脱,经HPLC-MS/MS测定,电喷雾离子源负离子模式检测,外标法定量。结果表明3种目标分析物在0.10~20.0 μg/L范围内线性关系良好,相关系数(r2)均大于0.999;蜂胶原胶、片剂和软胶囊剂型中3种目标物的检出限(LOD)为0.037~0.083 μg/kg,定量下限(LOQ)为0.12~0.28 μg/kg;硬胶囊剂型中的LOD为0.39~0.47 μg/kg,LOQ为1.28~1.57 μg/kg;在2.5、5.0、10.0 μg/kg加标水平下,3种目标物的回收率为66.6%~120%,相对标准偏差(RSD)为0.80%~11%。将该方法应用于45个实际样品检测,其中氯霉素的检出率为22.22%,最大残留量为14.32 μg/kg;氟甲砜霉素的检出率为17.78%,最大残留量为21.62 μg/kg。该方法操作简单、灵敏度高、适用性强,能够满足蜂胶、蜂胶原料保健食品中此类药物残留的检测要求。
中文关键词: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
 
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
Abstract: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.
Key Words:high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)  propolis  propolis derived dietary supplements  chloramphenicol  thiamphenicol  florfenicol
引用本文:杨黎,刘星,廖夏云,刘常凯,余仁连,苏小婷.高效液相色谱-串联质谱法同时测定蜂胶、蜂胶原料保健食品中的氯霉素、甲砜霉素与氟甲砜霉素[J].分析测试学报,2020,39(7):887-893.
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