CN105699166A - 一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法 - Google Patents

一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法 Download PDF

Info

Publication number
CN105699166A
CN105699166A CN201610259727.0A CN201610259727A CN105699166A CN 105699166 A CN105699166 A CN 105699166A CN 201610259727 A CN201610259727 A CN 201610259727A CN 105699166 A CN105699166 A CN 105699166A
Authority
CN
China
Prior art keywords
extraction
andrographis
andrographalide
dehydroandrographolide
extracting
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201610259727.0A
Other languages
English (en)
Inventor
陈学松
陈江涛
廖强
梁慧敏
李亚
李澄
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Wuzhou Institutes for Food and Drug Control
Original Assignee
Wuzhou Institutes for Food and Drug Control
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Wuzhou Institutes for Food and Drug Control filed Critical Wuzhou Institutes for Food and Drug Control
Priority to CN201610259727.0A priority Critical patent/CN105699166A/zh
Publication of CN105699166A publication Critical patent/CN105699166A/zh
Pending legal-status Critical Current

Links

Classifications

    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N1/00—Sampling; Preparing specimens for investigation
    • G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
    • G01N1/40—Concentrating samples
    • G01N1/4055—Concentrating samples by solubility techniques
    • G01N2001/4061—Solvent extraction
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N2030/022—Column chromatography characterised by the kind of separation mechanism
    • G01N2030/027—Liquid chromatography
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
    • G01N30/02—Column chromatography
    • G01N30/04—Preparation or injection of sample to be analysed
    • G01N30/06—Preparation
    • G01N2030/062—Preparation extracting sample from raw material

Abstract

本发明提供了一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法，旨在提供一种操作简单，提取完全，提取效率高的萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法；该方法是取样品粉末1g，置于10mL萃取池中，用甲醇对样品在温度60℃，静态提取5min，重复提取2次，提取完成后将提取液，合并两次提取液，减压蒸干即得；属于化学提取技术领域。

Description

一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法
技术领域
本发明提供一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法，属于化学萃取技术领域。
背景技术
穿心莲片收载于《中国药典》2005年版一部，其检查项为片剂制剂通则中规定的内容。中药口服固体制剂多以药物粉末或提取物为材料，有效成分必须通过崩解及溶出的过程释放，吸收进入血液而起到治疗作用。
发明内容
针对上述不足，本发明的目的是提供一种操作简单，提取完全，提取效率高的萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法。
为解决上述技术问题，本发明提供的技术方案如下：
一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法，该方法依次包括下述步骤：取样品粉末1g，置于10mL萃取池中，用甲醇对样品在温度60℃，静态提取5min，重复提取2次，提取完成后将提取液，合并两次提取液，减压蒸干即得。
进一步的，上述的一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法，所述的萃取仪为ASE350。
与现有技术相比，与现有技术相比，本发明提供的技术方案提取效率高，提取完全，可重复性好，方便后续检测，有利于控制产品质量。
具体实施方式
下面结合具体实施方式，对本发明的权利要求做进一步的详细说明，但不构成对本发明的任何限制，任何在本发明权利要求保护范围所做的有限次的修改，仍在本发明的权利要求保护范围之内。
本发明所涉及的到百分含量浓度，除特殊说明外，溶质为液体的均为体积浓度，溶质为固体的均为质量浓度。
实施例1
一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法，该方法依次包括下述步骤：取样品粉末1g，置于10mL萃取池中所述的萃取仪为ASE350，用甲醇对样品在温度60℃，静态提取5min，重复提取2次，提取完成后将提取液，合并两次提取液，减压蒸干即得。
为了验证本发明提供的技术方案：
去上述提取物1g，用甲醇定容至20mL，吸取1mL于离心管中，漩涡2min，10000r/min离心3min，收集上清液，混匀过0.22微米的滤膜，取滤液注入安捷伦Agilent-1200高效液相色谱仪进行检测。
所述的色谱条件如下：
色谱柱：StableBondSB-苯基柱(250mm×4.6mm，5μm)；
流动相：乙腈A-0.3％甲酸水溶液B；
流动相A为乙腈，流动相B为0.5％甲酸；梯度洗脱程序：0～1min，80％A、20％B；1～12min，85％～15％A、15％～85％B；12～15min，50％A、50％B；在50％A、50％B下平衡3min。
流速1mL/min；
波长：273nm，287nm；
柱温：35℃。
进样量:5μl。
对照品溶液:各取穿心莲内酯对照品、脱水穿心莲内酯对照品适量，加甲醇制成含穿心莲内酯16.6g.mL-1和脱水穿心莲内酯10.2g.mL-1的对照品混合溶液，按照相同方法进行检测，其谱图一直。

Claims (2)

1.一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法，其特征在于，该方法依次包括下述步骤：取样品粉末1g，置于10mL萃取池中，用甲醇对样品在温度60℃，静态提取5min，重复提取2次，提取完成后将提取液，合并两次提取液，减压蒸干即得。
2.根据权利要求1所述的一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法，其特征在于，所述的萃取仪为ASE350。
CN201610259727.0A 2016-04-25 2016-04-25 一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法 Pending CN105699166A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201610259727.0A CN105699166A (zh) 2016-04-25 2016-04-25 一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201610259727.0A CN105699166A (zh) 2016-04-25 2016-04-25 一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法

Publications (1)

Publication Number Publication Date
CN105699166A true CN105699166A (zh) 2016-06-22

Family

ID=56216452

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201610259727.0A Pending CN105699166A (zh) 2016-04-25 2016-04-25 一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法

Country Status (1)

Country Link
CN (1) CN105699166A (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106198781A (zh) * 2016-06-24 2016-12-07 广西灵峰药业有限公司 一种复方穿心莲片的生产质量控制方法

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1969895A (zh) * 2005-11-22 2007-05-30 徐小彬 穿心莲肠溶制剂及制备方法

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1969895A (zh) * 2005-11-22 2007-05-30 徐小彬 穿心莲肠溶制剂及制备方法

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
胡学桥等: "反相色谱法快速测定3种穿心莲内酯含量", 《合肥工业大学学报》 *
陈军辉 等: "加速溶剂萃取技术在中药有效成分分析中的应用", 《色谱》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106198781A (zh) * 2016-06-24 2016-12-07 广西灵峰药业有限公司 一种复方穿心莲片的生产质量控制方法

Similar Documents

Publication Publication Date Title
Zhang et al. Techniques for extraction and isolation of natural products: A comprehensive review
Rasul Extraction, isolation and characterization of natural products from medicinal plants
CN102621264A (zh) 一种含有人参皂苷类成分药材及制剂指纹图谱的建立方法
Kwon et al. Effect of processing method on platycodin D content in Platycodon grandiflorum roots
CN105085534B (zh) 一种生物碱化合物及其提取分离方法
CN105699166A (zh) 一种萃取穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法
CN102048906B (zh) 鸡骨草胶囊的含量测定方法
Lekar’ et al. Extraction of caftaric and cichoric acids from Echinacea purpurea L. in subcritical water
Liu et al. Optimization of supercritical fluid extraction of dl-tetrahydropalmatine from rhizome of Corydalis yanhusuo WT Wang with orthogonal array design
CN103211907A (zh) 四物汤复方配方颗粒及其制备方法和检测方法
CN105906687B (zh) 一种从丹参中分离纯化多种丹参酮单体成分的方法
CN105929066A (zh) Hplc测定穿心莲片中穿心莲内酯和脱水穿心莲内酯的方法
CN104297360B (zh) 一种复方血栓通制剂指纹图谱的检测方法
CN104892708A (zh) 从黄绿蜜环菌子实体规模化制备腺苷化学对照品的方法
CN105646638B (zh) 长梗冬青苷的制备方法
CN103044253A (zh) 一种藏丹参中迷迭香酸的提取分离方法
CN102692466A (zh) 济众酊的检测方法
CN107064325A (zh) 一种芪葛颗粒的质量控制方法
CN105699546A (zh) 液质串联法测定穿心莲片中有效成分含量的方法
CN105796619A (zh) 弱极性微球硅胶在三七总皂苷提取液浓缩中的用途
CN104147140A (zh) 一种秦皮配方颗粒的制备方法及其质量控制方法
CN103919885B (zh) 一种鼻渊软胶囊的制备方法及应用
Sunkar et al. Extraction and Purification of Bioactive Ingredients from Natural Products
CN107037165B (zh) 一种祖卡木制剂的质量检测方法
Hu et al. Applications of Pressurized Liquid Extraction in Quality Control of Traditional Chinese Medicines

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication
RJ01 Rejection of invention patent application after publication

Application publication date: 20160622