复方氨基酸注射液(18AA-Ⅱ)有关物质2-磺基色氨酸的研究

Study on the test of related substance 2-sulfonyltryptophan in compound amino acid injection(18AA-Ⅱ)

目的:建立HPLC法测定复方氨基酸注射液(18AA-Ⅱ)中2-磺基色氨酸的含量,并对2019年国家评价性抽验的国内7家企业155批产品进行分析。方法:采用Waters Atlantis T3色谱柱(250 mm×4.6 mm,5μm),以磷酸盐缓冲液-甲醇(94∶6)为流动相A,磷酸盐缓冲液-甲醇-乙腈(60∶6∶34)为流动相B,梯度洗脱,流速1.0 mL·min^(-1),柱温40℃,检测波长为220 nm,进样量10μL。结果:经方法学实验证明该测定方法准确可靠,2-磺基色氨酸在0.07~2.8μg·mL-1范围内其质量浓度与峰面积线性关系良好(Y=187014X+1093,r=1.000);加样回收率(n=9)为98.9%~102.9%,RSD为1.6%,连续进样精密度、溶液稳定性、专属性均良好。经方法学验证实验证明测定方法准确可靠,线性关系良好,回收率和灵敏度满足试验要求,精密度、稳定性、专属性均良好。结论:本法可以有效地测定复方氨基酸注射液(18AA-Ⅱ)中2-磺基色氨酸的含量,从而更好地控制复方氨基酸注射液类药品的质量。

Objective:To establish an HPLC method for determination of 2-sulfonyltryptophan in compound amino acid injection(18 AA-Ⅱ),and also to analyze the 155 batch products from 7 domestic enterprisesthat were selected for national drug evaluation sampling test in 2019.Methods:The determination was performed on an Waters Atlantis T3 column(250 mm×4.6 mm,5μm),with a mobile phase A consisting of phosphate buffer-methanol(94∶6)and mobile phase B consisting of phosphate buffer-methanol-acetonitrile(60∶6∶34)by gradient elution.The column temperature was set at 40℃with a flow rate of 1.0 mL·min^(-1).The detection wavelength was 220 nm.10μL aliquot was injected into HPLC for analysis.Results:The method was proved to be accurate and reliable.The linearity between concentration0.07-2.8μg·mL-1and peak area was good(Y=187014X+1093,r=1.000).The recovery rates were between 98.9%and 102.9%(n=9).RSD was 1.6%,the recovery ratesand sensitivity met the test requirements,precision,stability and specificity tests were all good.Conclusion:The method is validated to be useful for determination of content of related substance of 2-sulfonyltryptophan in compound amino acid injection(18 AA-Ⅱ),so asto better control the quality of compound amino acid injection drugs.