柴银口服液超高效液相色谱指纹图谱及6组分含量测定研究  

UPLC Fingerprint and Content Determination of Six Components in Chaiyin Oral Liquid

作　　者：关永霞 庄会芳 袁晓梅 金凤 庄建林 孙晓兰 白雪 范建伟 GUAN Yongxia;ZHUANG Huifang;YUAN Xiaomei;JIN Feng;ZHUANG Jianlin;SUN Xiaolan;BAI Xue;FAN Jianwei(Lunan Hope Pharmaceutical Co.,Ltd.,Linyi,Shandong,China 276006;Lunan Pharmaceutical Group Co.,Ltd.,State Key Laboratory of Generic Manufacture Technology of Chinese Traditional Medicine,Linyi,Shandong,China 276006)

机构地区：[1]鲁南厚普制药有限公司,山东临沂276006 [2]鲁南制药集团股份有限公司·中药制药共性技术国家重点实验室,山东临沂276006

出　　处：《中国药业》2022年第6期81-85,共5页China Pharmaceuticals

基　　金：山东省重点研发计划(重大科技创新工程)项目[2020CXGC010505];山东省临沂市兰山区科技创新发展计划专项[2026]。

摘　　要：目的建立柴银口服液的超高效液相色谱(UPLC)指纹图谱,并同时测定制剂中6个成分的含量。方法色谱柱为Waters Cortecs®C_(18)柱(50 mm×4.6 mm,2.7μm),流动相为乙腈-0.1%磷酸水溶液(梯度洗脱),检测波长为230 nm,流速为0.4~0.6 mL/min,柱温为35℃。以葛根素峰为参照峰,建立24批样品的UPLC图谱,采用“中药色谱指纹图谱相似度评价系统(2012版)”进行相似度评价,确定共有峰。结果24批样品UPLC图谱有30个共有峰,相似度均>0.97。葛根素、大豆苷、连翘酯苷A、黄芩苷、连翘苷、汉黄芩苷质量浓度分别在50.55~505.46μg/mL(r=0.9997)、11.20~112.04μg/mL(r=0.9996)、52.80~528.02μg/mL(r=0.9995)、149.01~1490.08μg/mL(r=0.9996)、12.41~124.10μg/mL(r=0.9996)、39.23~392.26μg/mL(r=0.9997)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验的RSD均小于2.0%;平均加样回收率分别为98.98%,98.51%,98.45%,98.43%,98.10%,98.86%,RSD分别为0.73%,1.07%,0.91%,0.82%,1.11%,0.73%(n=6)。结论所建立的UPLC指纹图谱结合含量测定,能更全面地表征柴银口服液的产品质量。Objective To establish the fingerprint of Chaiyin Oral Liquid by ultra-high performance liquid chromatography(UPLC),and to simultaneously determine the contents of six components in the preparation.Methods The chromatographic column was Waters Cortecs®C_(18) column(50 mm×4.6 mm,2.7μm),the mobile phase was acetonitrile-0.1%phosphoric acid solution(gradient elution),the detection wavelength was 230 nm,the flow rate was 0.4-0.6 mL/min,and the column temperature was 35℃.The UPLC fingerprint of 24 batches of samples were established with puerarin peak as the reference peak,and The Similarity Evaluation System of Chromatographic Fingerprints of Traditional Chinese Medicine(Version 2012)was used for similarity evaluation to determine the common peaks.Results There were 30 common peaks in the UPLC fingerprints of 24 batches of samples with the similarities all aboved 0.97.The linear ranges of puerarin,daidzin,forsythoside A,baicalin,forsythin and wogonoside were 50.55-505.46μg/mL(r=0.9997),11.20-112.04μg/mL(r=0.9996),52.80-528.02μg/mL(r=0.9995),149.01-1490.08μg/mL(r=0.9996),12.41-124.10μg/mL(r=0.9996),39.23-392.26μg/mL(r=0.9997),respectively.The RSDs of precision,stability and repeatability tests were less than 2.0%.The average recoveries of six components were 98.98%,98.51%,98.45%,98.43%,98.10%and 98.86%with RSDs of 0.73%,1.07%,0.91%,0.82%,1.11%and 0.73%(n=6),respectively.Conclusion The established UPLC fingerprint of content determination can more comprehensively characterize the product quality of Chaiyin Oral Liquid.

关 键 词：柴银口服液 超高效液相色谱法 指纹图谱 含量测定 

分 类 号：R932[医药卫生—生药学] R284.1[医药卫生—药学]