UPLC法快速测定生脉注射液及其中间体中5-羟甲基糠醛含量  

Rapid determination of 5-hydroxymethylfurfural in Shengmai Injection and its intermediates by UPLC

作　　者：聂黎行[1] 程显隆[1] 戴忠[1] 于健东[1] 马双成[1] NIE Li-xing;CHENG Xian-long;DAI Zhong;YU Jian-dong;MA Shuang-cheng(National Institutes for Food and Drug Control,Beijing 100050,China)

机构地区：[1]中国食品药品检定研究院,北京100050

出　　处：《时珍国医国药》2018年第9期2087-2089,共3页Lishizhen Medicine and Materia Medica Research

基　　金：国家自然科学基金(81303194);国家中医药管理局中药标准化建设项目(ZYBZH-C-JS-32);中国食品药品检定研究院学科带头人培养基金(2017X1)

摘　　要：目的采用超高效液相色谱技术建立生脉注射液及其中间体中5-羟甲基糠醛的快速限量检查方法。方法样品不经处理直接进样,经ACQUITY UPLC BEH C18色谱柱(2.1 mm×100 mm,1.8μm)分离,柱温35℃。甲醇-水(5∶95)洗脱,流速0.2 mL/min。检测波长284 nm。结果 5-羟甲基糠醛在0.002～0.2 mg/ml范围内线性关系良好,平均回收率为99.49%,RSD值为2.02%。7个厂家的18批生脉注射液中5-羟甲基糠醛含量在0.012～0.083 mg/ml之间,差别较大,同一厂家不同批次的样品测定结果差异不大。麦冬水提醇沉液和五味子水提醇沉液中5-羟甲基糠醛含量远高于红参醇提水沉液和五味子蒸馏液。结论所建方法准确、简便、快速,可为生脉注射液的质量控制和安全评价提供参考。Objective To establish a rapid limit test method of 5-hydroxymethylfurfural in Shengmai Injection and its intermediates by ultra-performance liquid chromatography（UPLC）.Methods The sample was injected directly without preprocessing.The separation was performed on an ACQUITY UPLC BEH C18 column（2.1 mm×100 mm,1.8 μm） and the column temperature was set at 35 ℃.The mobile phase was composed of methanol-water（5∶95） at a flaw rate of 0.2 mL/min.The detection wavelength was 284 nm.Results The calibration curve of 5-hydroxymethylfurfural showed good linearity within the range of 0.002～0.2 mg/mL.The average recovery was 99.49% with RSD of 2.02%.Contents of 5-hydroxymethylfurfural in 18 batches of Shengmai Injection from 7 manufactures varied from 0.012 to 0.083 mg/mL.And there were less variations among samples from the same manufacture.Contents of 5-hydroxymethylfurfural in water extraction and alcohol precipitation of Ophiopogonis Radix and water extraction and alcohol precipitation of Schisandrae Chinensis Fructus were much higher than those in alcohol extraction and water precipitation of Ginseng Radix et Rhizoma Rubra and distillate of Schisandrae Chinensis Fructus.Conclusion The proposed method was accurate,simple and rapid,thus providing basis for quality control and safety evaluation of Shengmai Injection.

关 键 词：生脉注射液 5-羟甲基糠醛(5-HMF) 中间体 超高效液相色谱(UPLC) 

分 类 号：R284.1[医药卫生—中药学]