对2015年版《中国药典》(一部)板蓝根【鉴别】(3)方法的改进
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摘要
目的:探讨2015年版《中国药典》(一部)(以下简称药典)中板蓝根【鉴别】(3)(R,S)-告依春薄层色谱(TLC)鉴别方法的合理性,并进行方法改进。方法:将3批板蓝根药材按药典板蓝根【炮制】方法制成饮片。首先按药典板蓝根【鉴别】(3)方法分别对板蓝根饮片和药材中(R,S)-告依春进行TLC鉴别(样品处理时以80%甲醇为溶剂,超声提取),考察药典方法的合理性。然后通过改变样品的提取溶剂及前处理方式(方法一:以水为溶剂,超声提取;方法二:先加水浸泡1 h,再加入甲醇超声提取;方法三:先将样品润湿,晾干后再以80%甲醇为溶剂,超声提取)进行方法改进,并对最优方法进行验证。最后按最优方法操作,分别采用不同厂家来源的色谱板,以及在低温低湿(7℃,相对湿度48%)和高温高湿(35℃,相对湿度75%)条件下进行(R,S)-告依春的TLC鉴别,考察方法的耐用性。结果:按药典方法进行检测,在饮片色谱中,与对照品色谱相应位置上显相同颜色的斑点,但在药材色谱中无相应斑点出现。按3种改进方法对样品进行处理后,在药材色谱中,与对照品色谱相应位置上均显相同颜色的斑点;但按方法一处理后色谱斑点单一,按方法二、三处理后色谱斑点均较多,且方法二较方法三耗时更短。验证试验结果和方法耐用性试验结果均显示,按方法二对板蓝根药材和饮片进行处理后,在饮片和药材色谱中,在与对照品色谱相应的位置上均显相同颜色的斑点。结论:改进后的TLC鉴别方法效果良好,色谱斑点清晰、重复性好。
OBJECTIVE: To investigate the rationality of TLC identification method(3) of(R,S)-epigoitrin in Isatis indigotica stated in 2015 edition of Chinese Pharmacopeia(part Ⅰ)(later abbreviated as pharmacopeia),and make some improvements. METHODS: Three batches I. indigotica were collected and prepared into decoction pieces according to the processing method of I. indigotica in pharmacopoeia. TLC identification of(R,S)-goitrin in I. indigotica decoction piece and medicinal material were conducted according to identification method(3) in pharmacopeia(80% ethanol as solvent for sample treatment,ultrasound extraction);the rationality of pharmacopoeia method was investigated. Then the method was improved by changing the extraction solvent and pretreatment method(method one:using water as solvent,ultrasound extraction;method two:soaking in water for 1 h,then adding into methanol,ultrasound extraction;method three:the sample was wetted and then dried,using 80% methanol as solvent,ultrasound extraction)of samples,and the optimal method was verified. According to the optimal method,the TLC identification of(R,S)-goitrin was detected by using chromatographic plates from different manufacturers,under the conditions of low temperature and low humidity(7 ℃,relative humidity 48%) and high temperature and high humidity(35 ℃,relative humidity 75%)respectively,to investigate the durability of the method. RESULTS:According to the method of pharmacopeia,in the chromatograms of decoction pieces,the same color spots appeared at the corresponding chromatographic positions of reference substance,but no corresponding spots appeared in the medicinal material chromatograms. After the samples were treated by three improvement methods, in medicinal material chromatograms, the same color spots appeared in the corresponding chromatographic positions of reference substances. There were single chromatographic spot after medicinal materials were treated with method one,and there were more spots after medicinal materials were treated with method two and three,and method two consumed less time than method three. The results of validation tests and method durability tests showed that after the treatment of I. indigotica and its decoction pieces according to method two,the same color spots appeared in the corresponding positions of the decoction pieces and the medicinal materials chromatograms as those of the control. CONCLUSIONS:The improved TLC identification method is effective, the chromatographic spots are clear,and the repeatability is good.
OBJECTIVE: To investigate the rationality of TLC identification method(3) of(R,S)-epigoitrin in Isatis indigotica stated in 2015 edition of Chinese Pharmacopeia(part Ⅰ)(later abbreviated as pharmacopeia),and make some improvements. METHODS: Three batches I. indigotica were collected and prepared into decoction pieces according to the processing method of I. indigotica in pharmacopoeia. TLC identification of(R,S)-goitrin in I. indigotica decoction piece and medicinal material were conducted according to identification method(3) in pharmacopeia(80% ethanol as solvent for sample treatment,ultrasound extraction);the rationality of pharmacopoeia method was investigated. Then the method was improved by changing the extraction solvent and pretreatment method(method one:using water as solvent,ultrasound extraction;method two:soaking in water for 1 h,then adding into methanol,ultrasound extraction;method three:the sample was wetted and then dried,using 80% methanol as solvent,ultrasound extraction)of samples,and the optimal method was verified. According to the optimal method,the TLC identification of(R,S)-goitrin was detected by using chromatographic plates from different manufacturers,under the conditions of low temperature and low humidity(7 ℃,relative humidity 48%) and high temperature and high humidity(35 ℃,relative humidity 75%)respectively,to investigate the durability of the method. RESULTS:According to the method of pharmacopeia,in the chromatograms of decoction pieces,the same color spots appeared at the corresponding chromatographic positions of reference substance,but no corresponding spots appeared in the medicinal material chromatograms. After the samples were treated by three improvement methods, in medicinal material chromatograms, the same color spots appeared in the corresponding chromatographic positions of reference substances. There were single chromatographic spot after medicinal materials were treated with method one,and there were more spots after medicinal materials were treated with method two and three,and method two consumed less time than method three. The results of validation tests and method durability tests showed that after the treatment of I. indigotica and its decoction pieces according to method two,the same color spots appeared in the corresponding positions of the decoction pieces and the medicinal materials chromatograms as those of the control. CONCLUSIONS:The improved TLC identification method is effective, the chromatographic spots are clear,and the repeatability is good.
引文
[1]国家药典委员会.中华人民共和国药典:一部[S].2015年版.北京:中国医药科技出版社,2015:205-206.
[2]马俊梅.板蓝根的现代药理及临床新用分析[J].中国卫生标准管理,2016,5(6):65-66.
[3]刁燕春.浅析板蓝根在临床诊疗中的应用效果[J].中医临床研究,2014,6(31):21-22.
[4]潘以琳,陈翰,李进,等.板蓝根药效活性部位化学成分的研究[J].中成药,2014,36(4):780-785.
[5]何立巍,董伟,杨婧妍,等.板蓝根抗病毒有效部位的化学成分及其活性研究[J].中草药,2013,44(21):2960-2964.
[6]杨建昕,李峰,李娜,等.板蓝根抗病毒活性成分研究进展[J].辽宁中医药大学学报,2016,18(7):141-143.
[7]国家药典委员会.中华人民共和国药典:一部[S].1985年版.北京:中国医药科技出版社,1985:169.
[8]何立巍,吴晓培,杨婧妍,等.板蓝根总生物碱的提取纯化工艺及其抗病毒药理作用研究[J].中成药,2014,36(12):2611-2614.
[9]王璐,戴敬,牛小莲.HPLC法测定清开灵软胶囊中(R,S)-告依春的含量[J].中国药房,2013,24(28):2764-2765.
[10]张文懿,李居安,杨天寿,等.不同采收期板蓝根的质量考察[J].中国药房,2009,20(27):2145-2147.
[11]冯家龙.HPLC法测定小儿清热止咳口服液中(R,S)-告依春的含量[J].中国药房,2013,24(40):3825-3827.
[12]王亚琦,葛秀允.板蓝根饮片产地加工炮制技术研究[J].中国药房,2018,29(5):656-658.
[13]国家药典委员会.中华人民共和国药典:一部[S].2010年版.北京:中国医药科技出版社,2010:191.
[14]莫迎.不同的提取方法对板蓝根中(R,S)-告依春的影响[J].中医药导报,2011,17(6):89-91.
[15]潘遐,刘效瑞,王兴政,等.板蓝根新品系品质考察及板蓝根质量标准改进[J].现代中药研究与实践,2015,29(3):66-69.
[16]徐丽华,黄芳,陈婷,等.板蓝根中的抗病毒活性成分[J].中国天然药物,2005,3(6):359-360.
[2]马俊梅.板蓝根的现代药理及临床新用分析[J].中国卫生标准管理,2016,5(6):65-66.
[3]刁燕春.浅析板蓝根在临床诊疗中的应用效果[J].中医临床研究,2014,6(31):21-22.
[4]潘以琳,陈翰,李进,等.板蓝根药效活性部位化学成分的研究[J].中成药,2014,36(4):780-785.
[5]何立巍,董伟,杨婧妍,等.板蓝根抗病毒有效部位的化学成分及其活性研究[J].中草药,2013,44(21):2960-2964.
[6]杨建昕,李峰,李娜,等.板蓝根抗病毒活性成分研究进展[J].辽宁中医药大学学报,2016,18(7):141-143.
[7]国家药典委员会.中华人民共和国药典:一部[S].1985年版.北京:中国医药科技出版社,1985:169.
[8]何立巍,吴晓培,杨婧妍,等.板蓝根总生物碱的提取纯化工艺及其抗病毒药理作用研究[J].中成药,2014,36(12):2611-2614.
[9]王璐,戴敬,牛小莲.HPLC法测定清开灵软胶囊中(R,S)-告依春的含量[J].中国药房,2013,24(28):2764-2765.
[10]张文懿,李居安,杨天寿,等.不同采收期板蓝根的质量考察[J].中国药房,2009,20(27):2145-2147.
[11]冯家龙.HPLC法测定小儿清热止咳口服液中(R,S)-告依春的含量[J].中国药房,2013,24(40):3825-3827.
[12]王亚琦,葛秀允.板蓝根饮片产地加工炮制技术研究[J].中国药房,2018,29(5):656-658.
[13]国家药典委员会.中华人民共和国药典:一部[S].2010年版.北京:中国医药科技出版社,2010:191.
[14]莫迎.不同的提取方法对板蓝根中(R,S)-告依春的影响[J].中医药导报,2011,17(6):89-91.
[15]潘遐,刘效瑞,王兴政,等.板蓝根新品系品质考察及板蓝根质量标准改进[J].现代中药研究与实践,2015,29(3):66-69.
[16]徐丽华,黄芳,陈婷,等.板蓝根中的抗病毒活性成分[J].中国天然药物,2005,3(6):359-360.