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引用本文:吴怀秀,王军娟,胡剀,宋珊珊,王向军.RRLC-QTOF鉴定拉科酰胺的未知杂质[J].中国现代应用药学,2014,31(5):563-566.
WU Huaixiu,WANG Junjuan,HU Kai,SONG Shanshan,WANG Xiangjun.RRLC-QTOF Applied to the Impurities Profile of Lacosamide[J].Chin J Mod Appl Pharm(中国现代应用药学),2014,31(5):563-566.
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RRLC-QTOF鉴定拉科酰胺的未知杂质
吴怀秀1, 王军娟2, 胡剀3, 宋珊珊3, 王向军1,3
1.浙江农林大学林业与生物技术学院,浙江 临安 311300;2.杭州宝荣科技有限公司,杭州 310030;3.浙江九洲药业股份有限公司,浙江 台州 318000
摘要:
目的 通过快速液相-四极杆飞行时间串联质谱(RRLC-QTOF)法分离、鉴定拉科酰胺粗品中4个未知杂质。方法 采用美国Agilent RRLC快速液相色谱系统和6530型四极杆-飞行时间串联质谱仪,色谱柱为XDB-C18(150 mm×4.6 mm,5 μm),流动相为醋酸铵-水溶液(甲酸调节pH至4.5)和乙腈,梯度洗脱,流速为1.0 mL·min-1,采用柱后分流,其中质谱仪进样流速为0.3 mL·min-1。结果 结合高分辨质量数和二级质谱碎片推测得到了拉科酰胺粗品中4个可能的杂质结构。结论 本研究为拉科酰胺的质量研究提供参考。
关键词:  拉科酰胺  杂质  四极杆-飞行时间质谱仪
DOI:
分类号:R917.101
基金项目:
RRLC-QTOF Applied to the Impurities Profile of Lacosamide
WU Huaixiu1, WANG Junjuan2, HU Kai3, SONG Shanshan3, WANG Xiangjun1,3
1.School of Forestry and Bio-technology, Zhejiang A&F University, Lin’an 311300, China;2.Hangzhou Baorong Science and Technology Co.,Ltd, Hangzhou 310051, China;3.Zhejiang Jiuzhou Pharmaceutical Co., Ltd, Taizhou 318000, China
Abstract:
OBJECTIVE To study the impurities profile of lacosamide with RRLC-QTOF method. METHODS The high performance liquid chromatography and quadrupole-flight time tandem mass spectrum (RRLC-QTOF) were used to analyze lacosamide. The column was XDB-C18(150 mm×4.6 mm, 5 μm). Acetonitrile and ammonium acetate buffer (pH4.5) were used as mobile phase with gradient elution. The total flow was 1 mL·min-1 and 0.3 mL·min-1 flowing into mass spectrum by a joint. RESULTS Combined the high resolution mass and MS2 fragment ions, the possible structure of four impurities in lacosamide were infered. CONCLUSION It is good reference for the research of the impurities profile in lacosamide.
Key words:  lacosamide  impurity  Q-TOF
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