摘要
目的考察连栀矾溶液在不同储存条件下其所含主要活性成分的含量变化情况,为连栀矾溶液的应用及质量提升提供参考。方法采用Eclipse Agilent C18色谱柱(250 mm×4.6 mm,5μm),以0.1%磷酸水溶液-乙腈为流动相进行梯度洗脱,体积流量1.0 mL/min,检测波长238 nm,柱温25℃。建立连栀矾溶液化学成分指纹图谱分析方法,用于测定分析其在密封及非密封储存条件下主要活性成分随时间的变化情况。结果所建立并采用的连栀矾溶液HPLC指纹图谱的精密度、稳定性、重复性和加样回收率均符合要求,可用于连栀矾溶液化学成分的分析。2种储存条件下不同时间点的样品指纹图谱与对照指纹图谱相似度值均大于0.95;利用外标指认法及光谱特征分析共指认出连栀矾溶液中的9种活性成分,其中的生物碱类物质(包括非洲防己碱、表小檗碱、盐酸药根碱、盐酸黄连碱、盐酸巴马汀和盐酸小檗碱)在2种储存条件下均无显著变化,但环烯醚萜类化合物京尼平龙胆双糖苷和栀子苷含量显著降低,京尼平含量在前3个月增加但超过3个月后其含量有所降低。推测京尼平龙胆双糖苷及栀子苷能被溶液中的酶转化为京尼平,而京尼平也可能会被微生物产生的其他酶所降解。结论连栀矾溶液在6个月的储存时间内,仍然存在成分的转化,这可能与储存过程中相关酶的作用有关。为提高每批次产品的质量一致性,建议可采用新的终点判断方法并在发酵炮制结束后对其采取酶的灭活和灭菌处理。
Objective To study on changes of active components in Lianzhifan solution(LZF)under different storage conditions,which may provide a reference for the application and quality improvement of the LZF.Methods HPLC analysis was performed on Eclipse Agilent C18 column(250 mm×4.6 mm,5μm).The gradient elution was performed by the mobile phase consisting of acetonitrile and 0.1%formic acid aqueous with the flow rate of 1.0 mL/min,the detection wavelength was set at 238 nm,and the column temperature was 25℃.A fingerprint analysis method for the chemical composition of LZF was established to analyze the change of main active components with time under sealed and unsealed storage conditions.Results The precision,stability,repeatability and sample recovery of the HPLC fingerprint of LZF were all in accordance with the requirements,and can be used for the analysis of the chemical constituents of LZF.The similarity values of sample fingerprints and control fingerprints at different time points under both storage conditions were greater than 0.95;The nine chemical components in LZF were identified by using the external labeling method and spectral characteristic analysis.The content of alkaloids(columbamine,epiberberine,jatrorrhizine chloride,coptisine chloride,palmatine chloride,and berberine)did not change significantly under the two storage conditions.However,the content of the iridoids,genipin-1-β-D-gentiobioside and geniposide was significantly reduced,and the content of genipin was increased in the first 3 months but decreased after 3 months.It is speculated that genipin-1-β-D-gentiobioside and geniposide can be converted to genipin by the enzyme in solution,and genipin may be degraded by other enzymes produced by microorganisms.Conclusion During the six-month storage period,LZF still has a convert tendency,which may be caused by the action of enzymes produced by microbes.In order to improve the quality consistency of LZF product,it is recommended to adopt more scientific method to judge the endpoint and it is better to inactivate enzyme and sterilize after the end of the fermentation processing.
作者
叶羊
张晓喻
杜娟
薛艾莲
杨梅
谢洁
袁学刚
杨向东
YE Yang;ZHANG Xiao-yu;DU Juan;XUE Ai-lian;YANG-Mei;XIE Jie;YUAN Xue-gang;YANG Xiang-dong(College of Life Sciences,Sichuan Normal University,Chengdu 610101,China;College of Geography and Resource Sciences,Sichuan Normal University,Chengdu 610101,China;Intercontinental Hospital of Proctology and Gastroenterology,Chengdu 610000,China;Chengdu Anorectal Hospital,Chengdu 610015,China)
出处
《中草药》
CAS
CSCD
北大核心
2019年第23期5745-5752,共8页
Chinese Traditional and Herbal Drugs
基金
四川省科技厅应用基础计划项目（2017JY0345）
四川省中医药科学技术研究专项（2016Q075）
关键词
连栀矾溶液
储存
生物碱
环烯醚萜
HPLC
非洲防己碱
表小檗碱
盐酸药根碱
盐酸黄连碱
盐酸巴马汀
Lianzhifan solution
storage
alkaloids
iridoids
HPLC
columbamine
epiberberine
jatrorrhizine chloride
coptisine chloride
palmatine chloride
berberine
genipin-1-β-D-gentiobioside
geniposide
genipin
