2023年第4期广东化工第50卷总第486期www.gdchem.com·23·全自动固相萃取仪高浓度氯霉素样品残留清洗程序的研究肖健，谢承恩，洪海燕(广州市越秀区疾病预防控制中心，广东广州510055)[摘要]本研究建立了一种适用于全自动固相萃取仪的高浓度氯霉素样本残留清洗程序。用高浓度氯霉素样本提取液上机进行固相萃取，分别用甲醇和水对进样通道、注射泵和柱塞杆三个部位进行不同体积的清洗，然后对不同清洗方法的氯霉素残留量测定结果用t检验、方差分析、SNK-q检验进行数据分析，得出最优溶剂和清洗程序。结果表明，水作为清洗溶剂清洗效果比甲醇好，Fotector-02HT全自动固相萃取仪的主要残留部位为进样通道，当样品氯霉素含量为5000μg/kg时，依次使用15mL水和10mL甲醇清洗进样通道，10mL水和10mL甲醇清洗注射泵，10mL水和10mL甲醇清洗柱塞杆，氯霉素残留量为0.0771μg/kg，低于方法0.1μg/kg的检出限。该清洗程序清洗效果稳定，氯霉素残留量低，可满足高浓度氯霉素样品的残留清洗要求。[关键词]全自动固相萃取仪；氯霉素；清洗程序；超高效液相色谱-串联质谱[中图分类号]R155[文献标识码]A[文章编号]1007-1865(2023)04-0023-03TheStudyofCleaningProceduresforAutomatedSolidPhaseExtractionContaminatedbySamplesWhichContainingHighConcentrationsofChloramphenicolXiaoJian,XieChengen,HongHaiyan(GuangzhouYuexiuCenterforDiseaseControlandPrevention,Guangzhou510055,China)Abstract:Toestablishacleaningproceduresforautomatedsolidphaseextractioncontaminatedbysampleswhichcontaininghighconcentrationsofchloramphenicol.Theextractsolutionofsampleswhichcontaininghighconcentrationsofchloramphenicolwassolidphaseextractedoninstrument,thenwashedinjectionchannel,syringepumpandplungerrodbydifferentvolumeofmethanolandwaterseparately.Theresidualconcentrationofchloramphenicolwasdetectedandresultswereanalyzedbyt-test,ANOVAandSNK-qtesttofindoutthebestsolventandcleaningprocedure.Thecleaningeffectofwaterisbetterthanthatofmethanol.ThemainresidualpartofFotector-02HTautomatedsolidphaseextractionwastheinjectionchannel.Ifasamplewhichcontain5000μg/kgofchloramphenicolwassolidphaseextractedoninstrument,washedtheinjectionchannelwith15mLwaterand10mLmethanol,washedthesyringepumpwith10mLwaterand10mLme...
