UPLC-HRMS法同时测定α-核糖甲磺酸酯中D-甘露醇和双丙酮-甘露醇含量  

Simultaneous Determination of D-Mannitol and Diacetone Mannitol in α-Ribose Methyl Methanesulfonate by UPLC-HRMS

作　　者：李林喆 毛联岗 姚彤 刘梦婷 顾娜 季春伟 张珍明 李树安[2,4] LI Lin-zhe;MAO Lian-gang;YAO Tong;LIU Meng-ting;GU Na;JI Chun-wei;ZHANG Zhen-ming;LI Shuan(School of Marine Life and Fisheries,Jiangsu Ocean University,Lianyungang 222005,China;School of Chemical Engineering,Jiangsu Ocean University,Lianyungang 222005,China;JARI Pharmaceutical Co.,Ltd.,Lianyungang 222006,China;Jiangsu Institute of Marine Resources,Lianyungang 222005,China)

机构地区：[1]江苏海洋大学海洋生命与水产学院,江苏连云港222005 [2]江苏海洋大学化学工程学院,江苏连云港222005 [3]连云港杰瑞药业有限公司,江苏连云港222006 [4]江苏省海洋资源开发研究院,江苏连云港222005

出　　处：《化学试剂》2021年第1期63-67,共5页Chemical Reagents

基　　金：江苏省海洋资源开发研究院科研项目(JSIMR201916);江苏省优势学科建设工程资助项目(5511201901X);连云港市“花果山英才计划”科技副总项目(2019.12);江苏海洋大学博士启动基金项目(KQ16001);江苏省研究生科研与实践创新计划项目(KYCX19_2292,KYCX19_2269,KYCX19_2273);江苏省大学生创新项目(SD201911641104003)。

摘　　要：建立了同时测定盐酸吉西他滨合成原料α-核糖甲磺酸酯中杂质D-甘露醇和双丙酮-甘露醇含量的超高效液相色谱-高分辨质谱法。采用菲罗门Titank C_(18)色谱柱,以70%乙腈水溶液(甲酸调至pH 3.0)为流动相,流速0.9 mL/min,柱温45℃。质谱为电喷雾(ESI)离子源,正离子模式扫描,外标法定量。D-甘露醇和双丙酮-甘露醇分别在1.00~12.53、0.99~12.42μg/mL浓度范围内线性关系良好,相关系数r分别为0.999 8和0.997 9,平均加标回收率分别为100.9%和99.5%。方法快速便捷、专属性强、灵敏度高、重现性好、结果准确可靠。A method was established for the simultaneous determination of D-mannitol and diacetone mannitol in α-Ribose methyl methanesulfonate,a raw material for synthesis of Gemcitabine hydrochloride,by ultra performance liquid chromatography-high resolution mass spectrometry(UPLC-HRMS).The analysis was performed on a Titank C_(18) column by using 70% acetonitrile solution(pH 3.0) as mobile phase at a flow rate of 0.9 mL/min and a column temperature of 45 ℃.The mass spectrometry used electrospray ionization and positive ion scanning mode.The contents were calculated by external standard method.The calibration curves for D-mannitol and diacetone mannitol showed good linearity in the ranges of 1.00~12.53 μg/mL and 0.99 ~12.42 μg/mL,with their correlation coefficients of 0.999 8 and 0.997 9,respectively.The average spiked recoveries for D-mannitol and diacetone mannitol were 100.9% and 99.5%,respectively.The method is efficient,convenient,sensitive,reproducible,accurate and reliable.

关 键 词：超高效液相色谱-高分辨质谱 盐酸吉西他滨 α-核糖甲磺酸酯 D-甘露醇 双丙酮-甘露醇 含量测定 

分 类 号：R917[医药卫生—药物分析学]