金英消食口服液的HPLC指纹图谱与含量测定研究(1)
【摘 要】 目的：建立金英消食口服液的HPLC指纹图谱及该制剂中橙皮苷含量测定的方法，为其质量控制提供依据。方法：采用HPLC法，用依利特Hypersil ODS2色譜柱(4.6 mm×250 mm，5 μm);以乙腈-0.1%磷酸水溶液(20∶ 80，V/V)为流动相;流速为1 mL/min;柱温为30 ℃;检测波长为283 nm。测定16批金英消食口服液的指纹图谱，并用国家药典委员“中药色谱指纹图谱相似度评价软件2012版”对其进行相似度评价;同时建立该制剂中橙皮苷的定量测定方法。结果：16批金英消食口服液的指纹图谱与对照指纹图谱的相似度均大于0.9;橙皮苷含量测定方法专属性好，精密度、稳定性、重现性等均符合方法学要求，且在一定范围内浓度与峰面积呈良好的线性关系。结论：所建立的指纹图谱和含量测定方法专属性好、稳定可靠，可用于金英消食口服液的质量控制。
【关键词】 高效液相色谱法;指纹图谱;橙皮苷;质量控制
【中图分类号】R284.1 【文献标志码】 A 【文章编号】1007-8517(2020)10-0051-06
Abstract：Objective To establish the HPLC fingerprint of Jinying Xiaoshi oral solution and determine the content of hesperidin， so as to provide a scientific basis for the quality control of Jinying Xiaoshi oral solution. Methods An HPLC method was used and the analysis was performed on an Hypersil ODS2 column(4.6 mm×250 mm，5 μm)using acetonitrile-0.1% phosphoric acid (20∶ 80，V/V) as mobile phase. The mobile phase flow rate was 1.0 mL·min-1.The temperature was 30 ℃.The detection wavelength was 283nm. The fingerprint of 16 batches of samples was tested and similarity evaluation was performed using Chinese Medicine Chromatographic Fingerprints Similarity Evaluation System software (2012).Besides， the content of hesperidin was determined. Results Totally 13 common peaks were identified in the fingerprint of Jinying Xiaoshi oral solution. The similarities between the 16 batches of samples and the reference fingerprint were all greater than 0.9.The method of quantitative analysis was established. The precision， stability and repeatability complied with the requirements of methodology. The standard curve of hesperidin had good linear relationship in ranges of the tested concentrations. Conclusion The HPLC fingerprint with high characteristics and the established content determination are stable， reliable and reproducible， which could be used for quality control of Jinying Xiaoshi oral solution.
Keywords：HPLC; Fingerprint; Hesperidin; Quality Control
金英消食口服液是太和县中医院临床应用多年的特色院内制剂，主要由鸡内金、麸炒白术、焦神曲、焦山楂、焦麦芽、姜半夏、蒲公英、陈皮、茯苓九药味组成。功能健胃醒脾、消食化滞，主要用于脾虚食滞所致的腹胀、纳呆、厌食、腹泻、小儿疳积。金英消食口服液作为质优价廉且临床应用多年的医院传统中药制剂，亟需建立完善的质量控制及评价方法，以保障制剂质量，为其进一步在临床推广应用奠定基础。实验通过高效液相色谱法建立金英消食口服液的指纹图谱和橙皮苷的含量测定方法，并制定橙皮苷的含量限度。
1 仪器与材料
UltiMate3000高效液相色谱仪(DAD检测器，赛默飞世尔科技有限公司); XP205DR型十万分之一分析天平(梅特勒-托利多仪器有限公司);KQ-500DE超声波清洗仪(昆山超声仪器有限公司)，万能粉碎机(上海贺帆仪器有限公司)。
对照品橙皮苷(批号：110721-201617，含量以96.1%计)购自中国食品药品检定研究院;乙腈、甲醇，均为色谱纯，美国天地公司;磷酸，分析纯，天津北方天医化学试剂厂;哇哈哈纯净水
金英消食口服液为太和县中医院中药制剂室生产，批号分别为20160511、20160513、20160515、20180510、20180606、20180720、20180731、20180808、20180818、20180821、20181005、20181007、20190104、20190117、20190306、20190430、20190726、20190810、20190906。缺味阴性样品均由中药制剂室自制。, http://www.100md.com(任莹 王虎 韩双)
【关键词】 高效液相色谱法;指纹图谱;橙皮苷;质量控制
【中图分类号】R284.1 【文献标志码】 A 【文章编号】1007-8517(2020)10-0051-06
Abstract：Objective To establish the HPLC fingerprint of Jinying Xiaoshi oral solution and determine the content of hesperidin， so as to provide a scientific basis for the quality control of Jinying Xiaoshi oral solution. Methods An HPLC method was used and the analysis was performed on an Hypersil ODS2 column(4.6 mm×250 mm，5 μm)using acetonitrile-0.1% phosphoric acid (20∶ 80，V/V) as mobile phase. The mobile phase flow rate was 1.0 mL·min-1.The temperature was 30 ℃.The detection wavelength was 283nm. The fingerprint of 16 batches of samples was tested and similarity evaluation was performed using Chinese Medicine Chromatographic Fingerprints Similarity Evaluation System software (2012).Besides， the content of hesperidin was determined. Results Totally 13 common peaks were identified in the fingerprint of Jinying Xiaoshi oral solution. The similarities between the 16 batches of samples and the reference fingerprint were all greater than 0.9.The method of quantitative analysis was established. The precision， stability and repeatability complied with the requirements of methodology. The standard curve of hesperidin had good linear relationship in ranges of the tested concentrations. Conclusion The HPLC fingerprint with high characteristics and the established content determination are stable， reliable and reproducible， which could be used for quality control of Jinying Xiaoshi oral solution.
Keywords：HPLC; Fingerprint; Hesperidin; Quality Control
金英消食口服液是太和县中医院临床应用多年的特色院内制剂，主要由鸡内金、麸炒白术、焦神曲、焦山楂、焦麦芽、姜半夏、蒲公英、陈皮、茯苓九药味组成。功能健胃醒脾、消食化滞，主要用于脾虚食滞所致的腹胀、纳呆、厌食、腹泻、小儿疳积。金英消食口服液作为质优价廉且临床应用多年的医院传统中药制剂，亟需建立完善的质量控制及评价方法，以保障制剂质量，为其进一步在临床推广应用奠定基础。实验通过高效液相色谱法建立金英消食口服液的指纹图谱和橙皮苷的含量测定方法，并制定橙皮苷的含量限度。
1 仪器与材料
UltiMate3000高效液相色谱仪(DAD检测器，赛默飞世尔科技有限公司); XP205DR型十万分之一分析天平(梅特勒-托利多仪器有限公司);KQ-500DE超声波清洗仪(昆山超声仪器有限公司)，万能粉碎机(上海贺帆仪器有限公司)。
对照品橙皮苷(批号：110721-201617，含量以96.1%计)购自中国食品药品检定研究院;乙腈、甲醇，均为色谱纯，美国天地公司;磷酸，分析纯，天津北方天医化学试剂厂;哇哈哈纯净水
金英消食口服液为太和县中医院中药制剂室生产，批号分别为20160511、20160513、20160515、20180510、20180606、20180720、20180731、20180808、20180818、20180821、20181005、20181007、20190104、20190117、20190306、20190430、20190726、20190810、20190906。缺味阴性样品均由中药制剂室自制。, http://www.100md.com(任莹 王虎 韩双)