液相色谱-质谱法测定甲磺酸多沙唑嗪中的磺酸酯  

Determination of Mesylate Esters in Doxazosin Mesylate by HPLC-Mass-Mass

作　　者：黄冰 陆超 程涛 张鑫鑫 Huang Bing;Lu Chao;Cheng Tao;Zhang Xinxin(Changzhou Pharmaceutical Factory,Changzhou 213018,China)

机构地区：[1]常州制药厂有限公司,江苏常州213018

出　　处：《山东化工》2023年第5期151-153,共3页Shandong Chemical Industry

摘　　要：目的:建立了衍生-液相色谱-质谱法测定甲磺酸多沙唑嗪中的甲磺酸甲酯、甲磺酸乙酯和甲磺酸丁酯。方法:采用2-巯基吡啶为衍生剂,采用Shim-pack GIST C_(18)(100 mm×2.1 mm, 2μm)色谱柱,结合梯度洗脱方式对样品进行分离,选择SIM和MRM模式,通过外标法定量。结果:方法在55~280 ng/mL质量浓度范围内具有良好的线性(r≥0.999),检测限为18×10~(-6),定量限为55×10~(-6);平均回收率在94.1%~117.6%,相对标准偏差为0.4%~6.4%。结论:该方法可用于检测甲磺酸多沙唑嗪中甲磺酸甲酯、甲磺酸乙酯和甲磺酸丁酯,方法专属强、结果准确、重现性好,可满足甲磺酸多沙唑嗪中甲磺酸酯的检测。Obiective:A derivative method of determination of methyl methanesulfonate(MMS),ethyl methanesulfonate(EMS)and butyl methanesulfonate(BMS)in doxazosin mesylate by HPLC-mass-msss was established.Methods:Using 2-Mercaptopyridine as the derivatization reagent,Shim-pack GIST C 18(100 mm×2.1 mm,2μm)chromatographic column,the sample was separated by gradient elution,selected by the mode of SIM and MRM,mesylate esters were quantified by the external standard method.Result:Mesylate esters have a good linear relationship in the range of 55~280 ng/mL(the correlation coefficient is not less than 0.999),the detection limit is 18×10-6 and the quantitative limit is 55×10-6,the recovery range was 93.3%~125.1%,and the relative standard deviation was 0.4%~6.4%.The method shows good specificity,accurate,and repeatability,which can satisfy the determination of mesylate esters in doxazosin mesylate.

关 键 词：甲磺酸多沙唑嗪 衍生 甲磺酸甲酯 甲磺酸乙酯 甲磺酸丁酯 液质联用仪 

分 类 号：O657.63[理学—分析化学]