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.
作者
李林喆
毛联岗
姚彤
刘梦婷
顾娜
季春伟
张珍明
李树安
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)
出处
《化学试剂》
CAS
北大核心
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)。
