高效液相色谱法测定环酯红霉素片的含量  

Determination of contents of erythromycin cyclocarbonate tablets using HPLC method

作　　者：侯金凤 李珉 黄晓春 寇晋萍 车宝泉 刘海涛 姚尚辰[2] HOU Jinfeng;LI Min;HUANG Xiaochun;KOU Jinping;CHE Baoquan;LIU Haitao;YAO Shangchen(Beijing Institute for Drug Control,NMPA Key Laboratory for Research and Evaluation of Generic Drugs,Beijing Key Laboratory of Analysis and Evaluation on Chinese Medicine,Beijing 102206,China;National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]北京市药品检验研究院,国家药品监督管理局仿制药研究与评价重点实验室,中药成分分析与生物评价北京市重点实验室,北京102206 [2]中国食品药品检定研究院,北京100050

出　　处：《中国药物警戒》2023年第11期1238-1242,共5页Chinese Journal of Pharmacovigilance

基　　金：国家重点研发计划(2022YFC3401205)。

摘　　要：目的建立高效液相色谱法测定环酯红霉素片的含量。方法将环酯红霉素片研细后,经乙腈提取,采用Waters XBridge C18(250 mm×4.6 mm,5μm)色谱柱,以0.02 mol·L^(-1)磷酸氢二钾溶液(用5 mol·L^(-1)氢氧化钾试液调节pH至11.4)-乙腈(35∶65)为流动相进行洗脱,流速为1.0 mL·min^(-1),在204 nm波长下测定。结果环酯红霉素在浓度0.51~1.52 mg·mL^(-1)范围内线性关系良好(r=0.9999),回收率在99.0%~100.5%(RSD为0.5%,n=9),重复性试验RSD为0.8%(n=6),中间精密度试验RSD为0.9%(n=12),供试品和对照品溶液5℃放置10h内均保持稳定,方法耐用性良好。3批供试品含量测定结果分别为102.3%、102.0%和103.5%,均在现行质量标准93.0%~107.0%限度范围内,符合规定。结论本方法操作简便、快速、准确、专属性好,适用于环酯红霉素片的含量测定,为该品种的深入研究提供了方法参考,为存在互变异构反应的化合物的液相色谱分析提供了研究思路。Objective To establish an HPLC method for determination of the content of erythromycin cyclocarbonate(EMC)tablets.Methods EMC tablets were grinded and extracted with acetonitrile.The chromatographic separation was performed on a Waters Xbridge C18 column(250 mm×4.6 mm,5μm)with an isocratic elution system composed of 0.02 mol·L-1 potassium hydrogen phosphate solution(adjust pH to 11.4 with 5 mol·L-1 potassium hydroxide solution)-acetonitrile(35:65)at a flow rate of 1.0 mL·min-1.The elutes were detected at the wavelength of 204 nm.Results A good linearity(r=0.9999)was observed within the range of 0.51 to 1.52 mg·mL-1.The recovery was between 99.0%and 100.5%(RSD=0.5%,n=9),the repeatability was 0.8%(n=6),and the intermediate precision was 0.9%(n=12).The test and standard sample solution remained stable for 10 hours at 5℃,and the method showed good durability.The contents of the three batches of EMC tablets were 102.3%,102.0%and 103.5%respectively,which were within the current standard limit range of 93.0%to 107.0%.Conclusion This method is simple,rapid,accurate and specific,and is workable for the content determination of EMC tablets.A reference method has become available for the in-depth study of EMC and for the analysis of compounds with tautomeric structure by liquid chromatography.

关 键 词：环酯红霉素 互变异构 含量测定 高效液相色谱法 

分 类 号：R971[医药卫生—药品] R744[医药卫生—药学]