摘要
目的建立快速测定复方甘草酸单铵系列注射剂中乙二胺四乙酸二钠(EDTA-2Na)含量的高效液相色谱(HPLC)法。方法色谱柱为Hypersil GOLD C_(18)柱(250 mm×4.6 mm,5μm),流动相为50 mmol/L磷酸二氢钠溶液(含5 mmol/L四丁基溴化铵,用磷酸溶液调pH至4.5)-乙腈(90∶10,V/V),流速为1.0 mL/min,检测波长为257 nm,柱温为40℃,进样量为10μL。结果EDTA-2Na质量浓度在2~200μg/mL范围内与EDTA-Fe3+线性关系良好(R^(2)=0.9998,n=7);检测限为0.02μg/mL,定量限为0.06μg/mL;精密度、重复性、稳定性试验的RSD均小于2.0%;复方甘草酸铵注射液、复方甘草酸单铵注射液、复方甘草酸单铵S氯化钠注射液、甘草酸单铵半胱氨酸氯化钠注射液、注射用复方甘草酸单铵S的平均回收率分别为100.57%,100.90%,100.86%,100.95%,101.03%,RSD分别为0.21%,0.82%,0.60%,0.64%,0.67%(n=9)。2家生产企业的样品中均未检出EDTA-2Na,7家生产企业的样品中EDTA-2Na含量均超出浓度(m/V)范围0.005%~0.1%,其他生产企业的样品中EDTA-2Na含量均在限定浓度范围内。结论该方法操作简便、重复性好、准确度高,可用于复方甘草酸单铵系列注射剂中EDTA-2Na的含量测定。各生产企业样品中EDTA-2Na添加量差异较大,其处方合理性有待提升。
Objective To establish a high-performance liquid chromatography(HPLC)method for the rapid determination of ethylenediaminetetraacetic acid disodium(EDTA-2Na)in Compound Ammonium Glycyrrhetate Series Injections.Methods The chromatographic column was Hypersil GOLD C_(18) column(250 mm×4.6 mm,5μm),the mobile phase was 50 mmol/L sodium dihydrogen phosphate solution(containing 5 mmol/L tetrabutylammonium bromide,pH was adjusted to 4.5 with phosphoric acid solution)-acetonitrile(90∶10,V/V),the flow rate was 1.0 mL/min,the detection wavelength was 257 nm,the column temperature was 40℃,and the injection volume was 10μL.Results The mass concentration of EDTA-2Na showed a good linear relationship with EDTA-Fe3+in the range of 2-200μg/mL(R^(2)=0.9998,n=7).The limit of detection(LOD)was 0.02μg/mL,and the limit of quantitation(LOQ)was 0.06μg/mL.The RSDs of precision,repeatability,and stability tests were lower than 2.0%.The average recoveries of Compound Ammonium Glycyrrhizin Injection,Compound Ammonium Glycyrrhetate Injection,Compound Ammonium Glycyrrhetate S and Sodium Chloride Injection,Compound Ammonium Glycyrrhetate Cysteine Sodium Chloride Injection,and Compound Ammonium Glycyrrhetate S for Injection were 100.57%,100.90%,100.86%,100.95%,and 101.03%with RSDs of 0.21%,0.82%,0.60%,0.64%,and 0.67%(n=9),respectively.No EDTA-2Na was detected in the samples from two manufacturers,and the content of EDTA-2Na in the samples from seven manufacturers exceeded the concentration(m/V)range of 0.005%-0.1%.The content of EDTA-2Na in the samples from other manufacturers was within the limited concentration range.Conclusion This method is simple,reproducible,and accurate,which can be used for the determination of EDTA-2Na in Compound Glycyrrhetate Series Injections.The additional amount of EDTA-2Na in samples from different manufacturers varies greatly,and its rationality needs to be further improved.
作者
路惬楠
田晓彤
王柳
张轶华
高燕霞
LU Qienan;TIAN Xiaotong;WANG Liu;ZHANG Yihua;GAO Yanxia(Hebei Institute for Drug and Medical Device Control·NDMA Key Laboratory for Quality Control and Evaluation of Generic Drug,Shijiazhuang,Hebei,China 050200)
出处
《中国药业》
CAS
2024年第1期83-87,共5页
China Pharmaceuticals
