摘要
目的:建立同时测定因卡膦酸二钠中磷酸三乙酯、亚磷酸二乙酯杂质含量的LC-MS/MS方法。方法:采用WATERS ACQUITYUPLC HSS C18分析柱(30 mm×2.1 mm,1.8μm),柱温为35℃,以0.1%甲酸水∶乙腈(7∶3,V/V)为流动相,流速为0.5 ml·min^(-1),进样体积为1μl。通过多反应离子监测模式(MRM)对磷酸三乙酯、亚磷酸二乙酯进行监测,其定量离子分别为m/z 127.1、m/z 111.1。结果:磷酸三乙酯与亚磷酸二乙酯分别在1.00~200.00 ng·ml^(-1)及3.30~200.00 ng·ml^(-1)检测范围内线性良好,线性相关系数r分别为0.9997,0.9999。分析方法的专属性、重复性、中间精密度、准确度、溶液稳定性、耐用性等验证参数均在2020版中国药典相应指导原则的规定范围内。结论:该LC-MS/MS定量方法准确度高、重复性好、耐用性强,可同时检测因卡膦酸二钠中磷酸三乙酯、亚磷酸二乙酯中的含量。
Objective:To develop and validate an LC-MS/MS method for the simultaneous determination of triethyl phosphate and diethyl phosphite in incadronate disodium.Methods:A WATERS ACQUITYUPLC HSS C18 column(30 mm×2.1 mm,1.8μm)was used,and the column temperature was set at 35℃.The mobile phase consisted of 0.1%formic acid water solution and acetonitrile(7∶3,V/V),the flow rate was 0.5 ml·min^(-1),and the injection volume was 1μl.By an MRM scanning mode,the quantitative ion of triethyl phosphate and diethyl phosphite was m/z 127.1 and m/z 111.1,respectively.Results:The linear range of triethyl phosphate and diethyl phosphite was 1.00-200.00 ng·ml^(-1)(r=0.9997)and 3.30-200.00 ng·ml^(-1)(r=0.9999),respectively.All the validation parameters for the method including specificity,repeatability,intermediate precision,accuracy,solution stability and durability were within the rangs of the corresponding guidelines in Chinese Pharmacopoeia(2020 edition).Conclusion:The LC-MS/MS method has the advantages of high accuracy,good repeatability and promising durability.It can be used for the simultaneous determination of triethyl phosphate and diethyl phosphite in incadronate disodium.
作者
黄伟静
黄伟民
陈伟翰
Huang Weijing;Huang Weimin;Chen Weihan(Guangzhou Daguang Pharmaceutical Co.Ltd.,Guangzhou 510535,China;Food and Drug Inspection Institute of Guangzhou Haizhu District)
出处
《中国药师》
CAS
2021年第5期981-984,共4页
China Pharmacist
