HPLC-CAD法同时测定牛磺罗定中的牛磺酰胺和牛磺酸  

Simultaneous Determination of Taurineamide and Taurine in Taurolidine by HPLC-CAD

作　　者：宗在伟[1] 盛晓玲 ZONG Zaiwei;SHENG Xiaoling(Jiangsu Aosaikang Pharmaceutical Co.,Ltd.,Nanjing 211112,China)

机构地区：[1]江苏奥赛康药业有限公司,南京211112

出　　处：《药学与临床研究》2024年第3期229-231,239,共4页Pharmaceutical and Clinical Research

摘　　要：目的:建立高效液相色谱法联合电喷雾式检测器(HPLC-CAD)同时测定4,4′-亚甲双[四氢-2H-1,2,4-噻二嗪]1,1,1′,1′-四氧化物(简称牛磺罗定)中两种工艺杂质[2-氨基乙烷磺酰胺(简称牛磺酰胺)和2-氨基乙磺酸(简称牛磺酸)]。方法:采用Sielc Primesep 500(4.6 mm×150 mm,5μm)为色谱柱,以10 mmol·L^(-1)甲酸铵(用甲酸调节pH值至3.4)(A)-乙腈(B)为流动相,梯度洗脱;流速1.0 mL·min^(-1),柱温20℃,CAD雾化器温度为35℃,进样量10μL。结果:牛磺酰胺和牛磺酸的线性范围分别为0.2254~3.0160μg·mL^(-1)(r=0.9991)和0.2212~2.9578μg·mL^(-1)(r=0.9993);平均加样回收率(n=9)分别为102.8%和101.8%,RSD分别为3.4%和2.2%。4批样品均未检出牛磺酰胺和牛磺酸。结论:根据ICH指南对所开发的方法进行了验证,结果表明,该方法具有良好的专属性、准确性和灵敏度,可用于牛磺罗定的质量控制。Objective:An HPLC-CAD method was developed to simultaneously determine impurities(taurineamide and taurine)in taurolidine.Methods:A Sielc Primesep 500 column(150 mm×4.6 mm,5μm)was used for separation in a gradient elution mode,with 10 mmol·L^(-1)ammonium formate solution(adjust to pH3.4 with formic acid)as mobile phase A and acetonitrile as mobile phase B.The flow rate was 1.0 mL·min^(-1).The column temperature was maintained at 20°C,the nebulization temperature of the detector was 35℃,and the injection volume was 10μL.Results:The method was determined to be linear in the range of 0.2254-3.0160μg·mL^(-1)(r=0.9991)for quantitation of taurineamide and 0.2212-2.9578μg·mL^(-1)(r=0.9993)for taurine.Method accuracy was assessed by spiking taurineamide and taurine at three levels.The average recoveries were 102.8%and 101.8%,with the RSDs of 3.4%and 2.2%,respectively.Conclusion:The developed method was validated as per ICH guideline and found to be specific,precise,sensitive and robust,which can be used for quality control of taurolidine.

关 键 词：牛磺罗定 牛磺酰胺 牛磺酸 电喷雾式检测器 高效液相色谱法 

分 类 号：R927[医药卫生—药学]