薄荷标准汤剂的指纹图谱及成分分析
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摘要
目的:建立薄荷标准汤剂的指纹图谱,并对其主要的共有峰进行成分归属,对其化学成分进行分析,并建立迷迭香酸的含量测定方法。方法:测定10批不同产地薄荷饮片水煎液制成的标准汤剂的HPLC指纹图谱,色谱条件为采用Kromasil 100-5-C_(18)色谱柱(4. 6 mm×250 mm,5μm),流动相乙腈-0. 2%甲酸水溶液梯度洗脱,柱温30℃,流速1 mL·min~(-1),检测波长330 nm。将10批指纹图谱导入"中药色谱指纹图谱相似度评价系统"(2012. 130723版),进行色谱峰匹配,采用平均数法生成对照图谱,并对10批指纹图谱进行相似度评价。结果:建立了薄荷饮片标准汤剂的指纹图谱,标定出13个共有峰;对10批不同产地薄荷饮片标准汤剂的指纹图谱进行相似度评价,相似度均达到0. 90以上;同时采用飞行时间质谱法对指纹图谱中的主要化学成分进行归属,并对其中9个共有峰进行了指认,使用该方法可同时测定迷迭香酸的含量。结论:该研究方法简单、准确、快速、重复性好、可行性强,能有效地对薄荷标准汤剂的质量进行快速评价,同时也为薄荷配方颗粒的质量评价奠定了基础。
Objective: To establish an HPLC fingerprint of Menthae Haplocalycis Herba standard decoction,in order to identify the main chemical component of common peaks, and determine the content of rosmarinic acid. Method: The chromatographic fingerprints of 10 batches of Menthae Haplocalycis Herba standard decoction from different areas were determined,and the chromatographic separation was carried out on Kromasil C_(18)( 4. 6 mm × 250 mm,5 μm) at the temperature of 30 ℃. The mobile phase was acetonitrile and 0. 1% formic acid solution for gradient elution,with a flow rate of 1 mL·min~(-1),and the detection wavelength was 330 nm. The10 batches of fingerprints were imported into Similarity Evaluation System for Chromatographic Fingerprint of TCM( 2012. 130723) for chromatographic peak matching,the reference fingerprint was established with the average method,and the similarities of 10 batches were evaluated. Result: The HPLC fingerprint of Menthae Haplocalycis Herba showed 13 common peaks. The similarities of 10 batches from different areas were all more than 0. 90. At the same time,9 common peaks of the fingerprint were identified by using Q-TOF-MS spectrometry. Rosmarinic acid content was also determined by using the HPLC fingerprint method. Conclusion: The method is simple,rapid and accurate,with a good reproducibility,and can be used to rapidly and effectively evaluate the quality of Menthae Haplocalycis Herba standard decoction and lay a foundation for the quality control of Menthae Haplocalycis Herba formula granules.
Objective: To establish an HPLC fingerprint of Menthae Haplocalycis Herba standard decoction,in order to identify the main chemical component of common peaks, and determine the content of rosmarinic acid. Method: The chromatographic fingerprints of 10 batches of Menthae Haplocalycis Herba standard decoction from different areas were determined,and the chromatographic separation was carried out on Kromasil C_(18)( 4. 6 mm × 250 mm,5 μm) at the temperature of 30 ℃. The mobile phase was acetonitrile and 0. 1% formic acid solution for gradient elution,with a flow rate of 1 mL·min~(-1),and the detection wavelength was 330 nm. The10 batches of fingerprints were imported into Similarity Evaluation System for Chromatographic Fingerprint of TCM( 2012. 130723) for chromatographic peak matching,the reference fingerprint was established with the average method,and the similarities of 10 batches were evaluated. Result: The HPLC fingerprint of Menthae Haplocalycis Herba showed 13 common peaks. The similarities of 10 batches from different areas were all more than 0. 90. At the same time,9 common peaks of the fingerprint were identified by using Q-TOF-MS spectrometry. Rosmarinic acid content was also determined by using the HPLC fingerprint method. Conclusion: The method is simple,rapid and accurate,with a good reproducibility,and can be used to rapidly and effectively evaluate the quality of Menthae Haplocalycis Herba standard decoction and lay a foundation for the quality control of Menthae Haplocalycis Herba formula granules.
引文
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[2]许一鸣,乐巍,桑梦如,等.不同产地薄荷药材商品质量及差异研究[J].中国中药杂志,2017,42(17):3391-3397.
[3]钟昆芮,张凡,姜艳艳,等.薄荷总黄酮的纯化工艺优选[J].中国实验方剂学杂志,2013,19(6):11-14.
[4]束雅春,段煜,陈亚军,等.薄荷-荆芥药对与单味药挥发性成分分析及体外抑菌作用比较[J].中国实验方剂学杂志,2019,25(7):6-13.
[5]国家药典委员会.关于征求《中药配方颗粒质量控制与标准制定技术要求(征求意见稿)》意见的通知[EB/OL]. http://www. chp. org. cn/view/ff808081559d1ea301565ac24962560d? a=XWJX.
[6]刘安.中药饮片标准汤剂制备与质量标准研究方法概述[J].中国实验方剂学杂志,2017,23(7):1.
[7]中华人民共和国国家中医药管理局.卫生部国家中医药管理局关于印发医疗机构中药煎药室管理规范的通知[EB/OL]. http://yzs. satcm. gov. cn/gongzuodongtai/2018-03-25/6577. html.
[8]陈向阳.薄荷酚类部位化学成分及抗炎活性研究[D].北京:北京中医药大学,2016.
[9]朱邵晴,朱振华,郭盛,等.不同干燥方法对薄荷药材中多元功效成分的影响与评价[J].中国中药杂志,2015,40(24):4860-4867.
[10]施树云,郭柯柯,彭胜,等. DPPH-HPLC-QTOF-MS/MS快速筛选和鉴定杜仲黑茶中抗氧化活性成分[J].天然产物研究与开发,2018,30(11):1913-1917.
[11]徐晶晶.基于抗氧化谱效关系分析的薄荷药材质量控制和评价方法研究[D].北京:北京中医药大学,2014.
[12]张昱,马惠玲,麦曦,等.基于UHPLC-Q-TOF-MS/MS技术鉴定薄荷在大鼠体内的入血成分及代谢产物[J].中草药,2017,48(19):3927-3934.
[13]马双刚,袁绍鹏,侯琦,等.山香圆叶中黄酮苷类成分及其抗炎活性研究[J].中国中药杂志,2013,38(11):1747-1750.