作者简介:刘静兰,硕士,主管药师。研究方向:药物分析。E-mail:lanjingliu0622@163.com作者单位:361012福建厦门,厦门市食品药品质量检验研究院HPLC法测定醋酸奥曲肽中醋酸和三氟乙酸的含量刘静兰[摘要]目的建立高效液相色谱法同时测定醋酸奥曲肽原料药中醋酸和三氟乙酸的含量。方法色谱柱为YMC-PackODS-AQ(4.6mm×250mm,5μm),流动相A为磷酸溶液(取磷酸7ml加水稀释至1000ml,混匀,用氢氧化铵溶液调节pH至3.0,再加入甲醇10ml,混匀),流动相B为甲醇,梯度洗脱,流速:1.0ml·min-1,检测波长:210nm,柱温:25℃。结果醋酸和三氟乙酸分别在10.092~1009.200μg·ml-1(r=1.0000)、0.496~49.570μg·ml-1(r=0.9999)范围内线性关系良好,定量限分别为30.9、16.6ng,检测限分别为10.9、7.0ng,平均回收率分别为99.78%、99.56%(n=9),RSD分别为0.36%、0.41%。结论该方法准确性高、专属性强、耐用性好,适用于测定醋酸奥曲肽中醋酸和三氟乙酸的含量。[关键词]醋酸奥曲肽;醋酸;三氟乙酸;高效液相色谱法[中图分类号]R917[文献标识码]A[文章编号]1008-9926(2023)4-0329-04[DOI]10.3969/j.issn.1008-9926.2023.04.012DeterminationofAceticAcidandTrifluoroaceticAcidinOctreotideAcetatebyHPLCLIUJing-lanXiamenInstituteforFoodandDrugControl,Xiamen361012,China[Abstract]ObjectiveToestablishanHPLCmethodforsimultaneousdeterminationofaceticacidandtrifluoroaceticacidinoctreotideacetate.MethodsTheHPLCgradientelutionmethodwasusedonaYMC-PackODS-AQcolumn(4.6mm×250mm,5μm)withphosphateacidsolution(7mlofphosphateacidwasdilutedwithwaterto1000ml,mixed,andpHwasadjustedto3.0withammoniumhydroxidesolutionbefore10mlofmethanolwasaddedandmixed)asmobilephaseA,andmethanolasmobilephaseBataflowrateof1.0ml·min-1.Thedetectionwavelengthwas210nmandthecolumntemperaturewas25℃.ResultsThelinearrangesofaceticacidandtrifluoroaceticacidwere10.092-1009.200μg·ml-1(r=1.0000)and0.496-49.570μg·ml-1(r=0.9999),respectively.Thelimitsofquantitationwere30.9ngand16.6ngrespectively,whilethoseofdetectionwere10.9and7.0ng,respectively.Theaveragerecoveries(n=9)were99.78%and99.56%,andtheRSDswere0.36%and0.41%,respective-ly.ConclusionThismethodisaccurate,specificanddurable,whichcanbeusedforthedeterminationofaceticacidandtrifluoroa...
