栀子不同部位栀子苷和西红花苷Ⅰ的提取工艺和含量测定
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摘要
为优选栀子不同部位中栀子苷和西红花苷Ⅰ的提取工艺并测定期含量,利用正交实验,采用超声、回流、微波3种方法,同时建立栀子苷和西红花苷Ⅰ的HPLC同步测定方法。结果表明,微波法的提取效果较好。果皮最佳提取工艺为提取温度为80℃,时间为25 min,料液比为1:15,乙醇浓度为95%;果仁最佳提取工艺为提取时间为30 min,料液比为1:20,温度为80℃,乙醇浓度为75%。采用Waters WATO54275-C18(4.6 mm×250 mm,5μm)色谱柱,以乙腈-0.1%磷酸水为流动相,流速为1 mL/min,进行梯度洗脱,栀子苷和西红花苷Ⅰ检测波长分别为238、440 nm。HPLC测定结果表明,‘林海1号’栀子果皮中栀子苷、西红花苷Ⅰ最高含量分别为13.53、3.3 mg/g;果仁中栀子苷、西红花苷Ⅰ最高含量分别为44.64、7.72 mg/g。上述结果为栀子种质评价和不同部位的开发利用提供科学参考和依据。
To optimize the extraction process, we used an orthogonal experiment to evaluate the extraction of geniposide and crocin I from different parts of gardenia by ultrasonic, reflux and microwave methods, and at the same time, established an HPLC method for simultaneous determination of these two components. The results showed that the extraction effect of the microwave method was the best. The optimum extraction process frompericarp was: extraction temperature was 80℃, time was 25 min, the ratio of material to liquid was 1:15,and the concentration of ethanol was 95%. The optimum extraction process from kernel was: the extractiontime of 30 min, the ratio of material to liquid of 1:20, the temperature of 80℃, and the concentration of ethanolof 75%. The HPLC separation was performed on a Waters WATO54275-C18(4.6 mm×250 mm, 5 μm) columneluted with the mobile phase of acetonitrile-0.1% phosphoric acid, the flow rate was 1 mL/min. The detectionwavelength of geniposide and crocin I was 238 and 440 nm. The HPLC results showed that the highest contentsof geniposide and crocetin I in the pericarp of gardenia‘Linhai-1'was 13.53 and 3.3 mg/g, respectively. Thehighest contents of geniposide and crocetin I in the kernel of gardenia‘Linhai-1'was 44.64 and 7.72 mg/g,respectively. The above results have certain reference value for the germplasm evaluation and the development and utilization of different parts of gardenia.
To optimize the extraction process, we used an orthogonal experiment to evaluate the extraction of geniposide and crocin I from different parts of gardenia by ultrasonic, reflux and microwave methods, and at the same time, established an HPLC method for simultaneous determination of these two components. The results showed that the extraction effect of the microwave method was the best. The optimum extraction process frompericarp was: extraction temperature was 80℃, time was 25 min, the ratio of material to liquid was 1:15,and the concentration of ethanol was 95%. The optimum extraction process from kernel was: the extractiontime of 30 min, the ratio of material to liquid of 1:20, the temperature of 80℃, and the concentration of ethanolof 75%. The HPLC separation was performed on a Waters WATO54275-C18(4.6 mm×250 mm, 5 μm) columneluted with the mobile phase of acetonitrile-0.1% phosphoric acid, the flow rate was 1 mL/min. The detectionwavelength of geniposide and crocin I was 238 and 440 nm. The HPLC results showed that the highest contentsof geniposide and crocetin I in the pericarp of gardenia‘Linhai-1'was 13.53 and 3.3 mg/g, respectively. Thehighest contents of geniposide and crocetin I in the kernel of gardenia‘Linhai-1'was 44.64 and 7.72 mg/g,respectively. The above results have certain reference value for the germplasm evaluation and the development and utilization of different parts of gardenia.
引文
[1]中国科学院中国植物志编辑委员会.中国植物志·第71卷[M].北京:科学出版社,1999:329.
[2](清)黄奭.神农本草经[M].北京:中医古籍出版社,1987:210.
[3]国家药典委员会.中华人民共和国药典[M].北京:中国医药科技出版社,2015:248-249.
[4]孟祥乐,李红伟,李颜,等.栀子化学成分及其药理作用研究进展[J].中国新药杂志,2011(11):959-967.
[5]龚庆宣.刘涓子.刘涓子鬼遗方[M].北京:人民卫生出版社,1986:23.
[6]王孝涛.历代中药炮制法汇典(古代部分)[M].南昌:江西科学技术出版社,1986:330-331.
[7]孙思邈.备急千金药方校释[M].北京:人民卫生出版社,1998:125,160,477.
[8]姚冬冬,舒娈,杨蕾,等.栀子苷降糖作用及相关机制研究[J].中草药,2014,45(8):1121-1125.
[9]王恩力,董方,姚景春.栀子苷药理学和毒理学研究进展[J].中国药房,2015,26(19):2730-2733.
[10]张耘实,祁贤,卢协勤,等.栀子苷对甲型H1N1流感病毒的抑制作用[J].中国药科大学学报,2016,47(2):204-209.
[11]方尚玲,刘源才,张庆华,等.栀子苷镇痛和抗炎作用的研究[J].时珍国医国药,2008,19(6):1374-1376.
[12]张红.栀子苷衍生物的合成及抗炎免疫活性研究[D].合肥:安徽医科大学,2013.
[13]程合理,赵新民.栀子苷的抗炎作用实验研究[J].安徽医药,2004(3):167-168.
[14]刘益华,李晶,林曼婷,等.栀子有效成分栀子苷的现代研究进展[J].中国药学杂志,2012,47(6):406-409.
[15]孙旭群,赵新民,杨旭.栀子苷利胆作用实验研究[J].安徽中医学院学报,2004(5):33-36.
[16]游伟良,平其能,孙敏捷,等.栀子苷的药理学研究新进展[J].药学进展,2012,36(4):158-162.
[17]王丽莎,梅妹.栀子苷对小鼠急性肺损伤保护机制的研究[J].中国农学通报,2012,28(23):26-31.
[18]陈雁,张现涛,张雷红,杨中林.栀子化学成分及药理作用研究进展[J].海峡药学,2010,22(12):1-5.
[19]韩宇,谢国勇,李冉,等.西红花苷药理活性的研究进展[J].现代药物与临床,2017,32(9):1806-1814.
[20]刘瑛,古天明,周红.西红花苷类成分药理作用研究概况[J].成都大学学报:自然科学版,2008,27(1):16-19.
[21]孙创斌,刘艳霞,刘国清,等.西红花苷的药理研究进展[J].西南国防医药,2011,21(8):914-916.
[22]绪广林,钱之玉.西红花苷对血管内皮细胞的保护作用研究[J].中草药,2002,33(5):439-442.
[23]张陆勇,周素娣.西红花总甙对鹌鹑实验性动脉粥样硬化的影响[J].中国药科大学学报,1999,30(5):383-386.
[24]刘涛.西红花苷的药理学研究进展[J].广东化工,2016,43(17):77-78.
[25]段李歌.食药两用栀子果的差异化质量评价及主要功效成分的分离纯化[D].武汉:武汉轻工大学,2014.
[2](清)黄奭.神农本草经[M].北京:中医古籍出版社,1987:210.
[3]国家药典委员会.中华人民共和国药典[M].北京:中国医药科技出版社,2015:248-249.
[4]孟祥乐,李红伟,李颜,等.栀子化学成分及其药理作用研究进展[J].中国新药杂志,2011(11):959-967.
[5]龚庆宣.刘涓子.刘涓子鬼遗方[M].北京:人民卫生出版社,1986:23.
[6]王孝涛.历代中药炮制法汇典(古代部分)[M].南昌:江西科学技术出版社,1986:330-331.
[7]孙思邈.备急千金药方校释[M].北京:人民卫生出版社,1998:125,160,477.
[8]姚冬冬,舒娈,杨蕾,等.栀子苷降糖作用及相关机制研究[J].中草药,2014,45(8):1121-1125.
[9]王恩力,董方,姚景春.栀子苷药理学和毒理学研究进展[J].中国药房,2015,26(19):2730-2733.
[10]张耘实,祁贤,卢协勤,等.栀子苷对甲型H1N1流感病毒的抑制作用[J].中国药科大学学报,2016,47(2):204-209.
[11]方尚玲,刘源才,张庆华,等.栀子苷镇痛和抗炎作用的研究[J].时珍国医国药,2008,19(6):1374-1376.
[12]张红.栀子苷衍生物的合成及抗炎免疫活性研究[D].合肥:安徽医科大学,2013.
[13]程合理,赵新民.栀子苷的抗炎作用实验研究[J].安徽医药,2004(3):167-168.
[14]刘益华,李晶,林曼婷,等.栀子有效成分栀子苷的现代研究进展[J].中国药学杂志,2012,47(6):406-409.
[15]孙旭群,赵新民,杨旭.栀子苷利胆作用实验研究[J].安徽中医学院学报,2004(5):33-36.
[16]游伟良,平其能,孙敏捷,等.栀子苷的药理学研究新进展[J].药学进展,2012,36(4):158-162.
[17]王丽莎,梅妹.栀子苷对小鼠急性肺损伤保护机制的研究[J].中国农学通报,2012,28(23):26-31.
[18]陈雁,张现涛,张雷红,杨中林.栀子化学成分及药理作用研究进展[J].海峡药学,2010,22(12):1-5.
[19]韩宇,谢国勇,李冉,等.西红花苷药理活性的研究进展[J].现代药物与临床,2017,32(9):1806-1814.
[20]刘瑛,古天明,周红.西红花苷类成分药理作用研究概况[J].成都大学学报:自然科学版,2008,27(1):16-19.
[21]孙创斌,刘艳霞,刘国清,等.西红花苷的药理研究进展[J].西南国防医药,2011,21(8):914-916.
[22]绪广林,钱之玉.西红花苷对血管内皮细胞的保护作用研究[J].中草药,2002,33(5):439-442.
[23]张陆勇,周素娣.西红花总甙对鹌鹑实验性动脉粥样硬化的影响[J].中国药科大学学报,1999,30(5):383-386.
[24]刘涛.西红花苷的药理学研究进展[J].广东化工,2016,43(17):77-78.
[25]段李歌.食药两用栀子果的差异化质量评价及主要功效成分的分离纯化[D].武汉:武汉轻工大学,2014.