固相萃取-高效液相色谱-串质谱法测定蜂胶中氯霉素残留  

Overcoming Lipophilic Interference in Propolis to Quantify Residual Chloramphenicol by Solid-Phase Extraction Coupled with Liquid Chromatography-Tandem Mass Spectrometry

作　　者：王玉涵 王欣然[1] 陆超丽 吴殿军 周金慧[1,3,4] 李熠 WANG Yu-han;WANG Xin-ran;LU Chao-li;WU Dian-jun;ZHOU Jin-hui;LI Yi(Institute of Apicultural Research,Chinese Academy of Agricultural Sciences,Beijing 100093,China;Rural Social Undertakings Promotion Station of Zhaoping County,Hezhou 546800,Guangxi,China;Laboratory of Risk Assessment for Quality and Safety of Bee Products,Ministry of Agriculture and Rural Affairs,Beijing 100093,China;Key Laboratory of Bee Products for Quality and Safety Control,Ministry of Agriculture and Rural Affairs,Beijing 100093,China;Institute of Food Science and Technoology,Chinese Academy of Agricultural Scievces,Beijing 100193,China)

机构地区：[1]中国农业科学院蜜蜂研究所,北京100093 [2]昭平县农村社会事业促进站,广西贺州546800 [3]农业农村部蜂产品质量安全控制重点实验室,北京100093 [4]农业农村部蜂产品质量安全风险评估实验室,北京100093 [5]中国农业科学院农产品加工研究所,北京100193

出　　处：《食品研究与开发》2022年第1期160-166,共7页Food Research and Development

基　　金：国家自然科学基金面上项目(32172305);国家蜂产业技术体系(CARS-44-KXJ8);国家特色农产品风险评估专项(GJFP2020010);中国农业科学院创新工程项目(CAAS-ASTIP-2020-IAR)。

摘　　要：该文建立固相萃取结合高效液相色谱-串联质谱技术(solid phase extraction-high performance liquid chromatography-tandem mass spectrometry,SPE-HPLC-MS/MS)测定蜂胶中氯霉素残留的检测方法。蜂胶样品经乙腈溶解,氢氧化钙溶液沉淀杂质,Bond Elut Plexa固相萃取柱(6mL,200mg)净化,Kinetex C18色谱柱(50mm×2.1mm,2.6μm)分离,以水-乙腈为流动相梯度洗脱分离,在负模式下,采用多反应监测(multiple reaction monitoring,MRM)模式检测,内标法定量。结果表明,氯霉素在0.1μg/L~500.0μg/L范围内线性关系良好(R2>0.99),检出限为0.4μg/kg,定量限为1.0μg/kg。氯霉素在蜂胶样品中添加水平为1、2、10μg/kg时平均回收率为93.2%~103.4%,日内和日间相对标准偏差分别为0.98%~3.95%和0.93%~5.37%(n=5)。该方法操作简便,耗时短,灵敏度高,稳定性好,适用于蜂胶中氯霉素残留筛查检测及定量分析。An approach using solid phase extraction-high performance liquid chromatography-mass spectrometry(HPLC-MS/MS)was developed for determination of chloramphenicol(CAP)residue in propolis. The propo lis samples were dissolved in acetonitrile,and then calcium hydroxide [Ca(OH)2] solution was added to break the lipophilic interferences. Solid phase extraction column(Bond Elut Plexa,6 mL,200 mg)was used to remove other impurities from propolis prior to HPLC-MS/MS analysis. The target compound was separated on Kinetex C18 column(50.0 mm×2.1 mm,2.6 μm)with mobile phase of water and acetonitrile.The quantitative detection was performed using an electrospray ionization source in negative ionization mode under multiple reaction monitoring(MRM).An isotopically labeled CAP(CAP-D5)as the internal standard was used to quantify CAP residue in propolis.The standard curve was constructed and exhibited a strong linear relationship(R2>0.99)in the range of 0.1 μg/L-500.0 μg/L. The limit of detection(LOD)for CAP in propolis was 0.4 μg/kg,and the limit of quantification(LOQ)was 1.0 μg/kg. The method was validated by analyzing samples spiked at three levels of 1,2,10 μg/kg. The recoveries ranged from 93.2% to 103.4%,intra-and inter-day precisionrelative standard deviation(RSD)ranged from 0.98% to 3.95% and 0.93% to 5.37%(n =5),respectively. The method was simple,rapid,sensitive and stable,whichis suitable to screen and quantify CAP residue in propolis.

关 键 词：氯霉素 蜂胶 高效液相色谱-串联质谱 固相萃取 残留测定 

分 类 号：O657.63[理学—分析化学] S896.6[理学—化学]