LC-MS%2fMS测定碘海醇及注射剂中有关物质研究.pdfVIP

LC．MS／MS测定碘海醇及其注射剂中有关物质的研究 刘菁1一，蔡梅2，谭力2，季红英3，石锦萍3，王玉1·2‘《I．中国药科大学．南京210009；2．江苏省食品药品检验所．南京 210008；3、扬子江药业集团质量部．江苏泰州225321 摘要：目的 建立液相色谱一串联质谱联用方法，对碘海醇及其注射剞中两种有关物质进行分离和测定．方法柱：Agilent CIB分析柱 150x4．6mm．3．5 用ESI离子化．串联质谱选择离子监测 SRM 正离子模式检测，喷雾电压：3500V，鞘气流速：30L·min～，辅助气流速： 5L·min一，毛细管温度：325℃，离子选择通道分别为m／z747．8／528．9 有关物质A ，m／z705．8／614．7 有关物质B 和 m／z ng·ml’1— 1080 lRSD：4．4％ 、105．2％ RSD：7．6％ ．结论法可同时测定碘海醇及其注射荆中的两种有关物质． 关键词：碘海醇；有关物质；LC．MS／MS SimultaneousDeterminationofTwoRelated inlohexolandits LC-MS／MS Compounds Injectionby LIU Mei2，TANLi2，JI Yul．2 1．ChinaPharmaceutical Jingu，CAI Hong．yin93，SHIJin．pin93，WANG 21 InstituteForFoodand River 21 Pharmaceutical University；Nanjing0008：2．diangsu DrugControl,Nanjing0008：3． bngtze Group, Taizhou225321 dmngsu A methodforthedeterminationof related iniohexolandits ABSTRACT：OBJECTB’ELC-MS／MS two compounds injection WaS An was withthe established used mobile ofacetonitrile firstly．METHODSAgilentC1l 150×4．6mm，3．5蝉m column phase andwater 0．05％formicflowratewas0．25ml·minq．thecolumn was was acid ．the temperature30℃．Sampleanalyzedby ionizationselectedreaction Wassetat3500 typc．111e V,transfer electrosprayapplying monitoring SRM scansprayvoltage capillary at and at30and5L‘min‘．neselectedionsformass 325℃，sheath temperature gas auxiliarygas nitrogen pressure monitoring m／z 1 m／z were 705．8／6 B and 11侍 747．8／528．9 relatedcompoundA ，m／z 4．7 relatedcompound 328．2／237．0 1S ．REStⅢT．s linear ofrelated AandBwere0．2818 26．90 ranges compound lag‘ml“～11．27¨g’ml～ r---0．9994 andng‘ml。～1080ng‘mL1 recoveriesofrelated AandBatthreelevelswere1 105．4％ average 03．2％ RSD：4．4％ and r O．9963 ，respectively．m compound TheestablishedLC-MS／MSmethodcan tworelated iniohexol RSD：7．8％ ，respectively．CONCLUSlON quantity compounds and its and injectionsimultaneouslyaccurately． KEYu70RDS．．iohexol·ralated compound：LC-MS／MS 碘海醇 Iohex01 化学名为5．【 N．2，3-二羟丙的研究不多，USPl2J中采用高效液相色谱法对碘海 醇及注射剂中有关物质进行检查和限量，陆豪杰等 基 乙酰胺基】-N，N’．双 2，3．二羟丙基 -2，4，6．三碘 一l，3．苯二甲酰胺