CN113406233A - 一种健脾壮腰药酒中阿魏酸和梓醇的含量测定方法 - Google Patents
一种健脾壮腰药酒中阿魏酸和梓醇的含量测定方法 Download PDFInfo
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Abstract
本发明涉及一种健脾壮腰药酒中阿魏酸和梓醇的含量测定方法,所述方法,包括方法1,阿魏酸的含量测定方法,其色谱条件为:色谱柱:Agilent ZORBAX SB‑C18(4.6*250mm*5μm);柱温:35℃;进样量:10μl;检测波长:316nm;流速:1ml/min;流动相:乙腈‑0.1%磷酸(16:84),阿魏酸应和相邻的色谱峰分离度>1.5;运行时间:50min;和方法2,梓醇含量测定方法,其色谱条件为:色谱柱:Agilent ZORBAX SB‑C18(4.6*250mm*5μm);柱温:30℃;进样量:10μl;波长:210nm;流速:0.8ml/min;流动相:甲醇‑0.1%磷酸(1:99)。
Description
技术领域
本发明涉及一种健脾壮腰药酒中阿魏酸和梓醇的含量测定方法。
背景技术
健脾壮腰药酒,
【处方】甘草10g红花10g山药30g地黄60g龙眼肉30g黄芪50g大枣80g制何首乌40g当归30g牛膝50g续断60g党参40g茯苓40g杜仲40g
【制法】以上十四味,以白酒4500g、4500g分二次浸渍,每2次星期,取上清滤,滤过,合并滤液。另取少量白酒加热溶化后,加入药酒搅匀,静置沉淀2~3星期取上清液,滤过,约得9450g,即得。
【性状】本品为红棕色澄清液;味甜、微苦。
健脾壮腰药酒具有补气养血,健脾补肾,通经活络的功效。用于气血不足,纳食不佳,腰腿酸楚,神疲乏力,失眠健忘。口服,一次20~30毫升,早晨及临睡前各服一次。
现有健脾壮腰药酒质量标准中仅有甘草、当归、红花、续断薄层鉴别方法和乙醇含量检测检测方法,尚未建立含量测定方法,随着对中药产品质量控制要求的提高,对于药物中的有效成分进行检测的要求也被提上日程,为此,有必要对健脾壮腰药酒中中药有效成分进行研究并建立含量测定方法。
现有文献报道中,陈岩仅对健脾壮腰药酒其中的主要药味甘草、红花、黄芪、当归、续断等进行了薄层色谱鉴别研究。孙莹莹等研究了益精丸中梓醇和阿魏酸的含量测定方法。
现有技术中未有公开健脾壮腰药酒中阿魏酸和梓醇的含量测定方法。本发明公开的健脾壮腰药酒中阿魏酸和梓醇的含量测定方法操作简单、专属性强、准确度高、结果可靠,可作为健脾壮腰药酒质量控制标准。
发明内容
本发明的目的旨在提供一种健脾壮腰药酒中阿魏酸和梓醇的含量测定方法。方法1,健脾壮腰药酒中阿魏酸的含量测定方法,包括以下步骤:
(1)阿魏酸对照品溶液的制备:取阿魏酸对照品适量,精密称定,加甲醇溶解制成溶液;
(2)供试品溶液的制备:吸取健脾壮腰药酒,过滤,即得;
(3)阴性溶液的制备:按照药酒处方制备不含当归药材的阴性溶液,过滤,即得;
(4)测定:分别精密吸取阴性溶液、阿魏酸对照品溶液及供试品溶液,注入液相色谱仪,得到色谱图,根据色谱图计算阿魏酸的含量。
优选的方法1,包括以下步骤:
(1)阿魏酸对照品溶液的制备:取阿魏酸对照品适量,精密称定,加60-800%甲醇溶解制成每1ml约含15-25μg的溶液,过滤,取续滤液,即得;
(2)供试品溶液的制备:吸取健脾壮腰药酒,过滤,取续滤液,即得;
(3)阴性溶液的制备:按照药酒处方制备不含当归药材的阴性溶液,过滤,取续滤液,即得;
(4)测定:分别精密吸取阴性溶液、阿魏酸对照品溶液及供试品溶液各5-20μl,注入液相色谱仪,得到色谱图,根据色谱图计算阿魏酸的含量。
最优选的方法1,包括以下步骤:
(1)阿魏酸对照品溶液的制备:取阿魏酸对照品适量,精密称定,加70%甲醇溶解制成每1ml约含20μg的溶液,过0.22μm的滤膜,取续滤液,即得;
(2)供试品溶液的制备:吸取健脾壮腰药酒3ml,过0.22μm的滤膜,取续滤液,即得;
(3)阴性溶液的制备:按照药酒处方制备不含当归药材的阴性溶液,过0.22μm的滤膜,取续滤液,即得;
(4)测定:分别精密吸取阴性溶液、阿魏酸对照品溶液及供试品溶液各10μl,注入液相色谱仪,得到色谱图,根据色谱图计算阿魏酸的含量。
色谱条件:
色谱柱:Agilent ZORBAX SB-C18(4.6*250mm*5μm);柱温:35℃;进样量:10μl;检测波长:316nm;流速:1ml/min;流动相:乙腈-0.1%磷酸(16:84),阿魏酸应和相邻的色谱峰分离度>1.5;运行时间:50min。
方法2,健脾壮腰药酒中梓醇含量测定方法,包括以下步骤:
(1)梓醇对照品溶液的制备:取梓醇对照品适量,精密称定,加磷酸制成溶液,即得;
(2)供试品溶液的制备:取健脾壮腰药酒适量,过滤,即得;
(3)阴性溶液的制备:按照药酒处方制备不含地黄药材的阴性溶液,过滤,即得;(4)测定:测定:分别精密吸取阴性溶液、梓醇对照品溶液及供试品溶液注入液相色谱仪,得到色谱图,根据色谱图计算梓醇的含量。
优选的方法2,包括以下步骤:
(1)梓醇对照品溶液的制备:取梓醇对照品适量,精密称定,加0.08-0.12%的磷酸制成每1ml约含0.08-0.12mg的溶液,即得。
(2)供试品溶液的制备:取健脾壮腰药酒适量,过滤,取续滤液,即得;
(3)阴性溶液的制备:按照药酒处方制备不含地黄药材的阴性溶液,过滤,取续滤液,即得;
(4)测定:测定:分别精密吸取阴性溶液、梓醇对照品溶液及供试品溶液各5-20μl,注入液相色谱仪,得到色谱图,根据色谱图计算梓醇的含量。
最优选的方法2,包括以下步骤:
(1)梓醇对照品溶液的制备:取梓醇对照品适量,精密称定,加0.1%磷酸解制成每1ml约含0.1mg的溶液,即得。
(2)供试品溶液的制备:取健脾壮腰药酒适量,用0.22μm滤膜过滤,取续滤液,即得;
(3)阴性溶液的制备:按照药酒处方制备不含地黄药材的阴性溶液,过0.22μm的滤膜,取续滤液,即得;
(4)测定:测定:分别精密吸取阴性溶液、梓醇对照品溶液及供试品溶液各10μl,注入液相色谱仪,得到色谱图,根据色谱图计算梓醇的含量。
色谱条件:
色谱柱:Agilent ZORBAX SB-C18(4.6*250mm*5μm);柱温:30℃;进样量:10μl;波长:210nm;流速:0.8ml/min;流动相:甲醇-0.1%磷酸(1:99)。本发明是经过筛选得到的,筛选过程如下:
阿魏酸的含量测定:流动相从不同比例乙腈-水,筛选更换为乙腈-0.1%磷酸,再对乙腈和0.1%的磷酸比例进行了筛选,从12:88,15:85,16:84,最终优化确定为17:83,阿魏酸和其他干扰成分获得良好的分离。
梓醇的含量测定:对供试品溶液的提取进行了筛选,先采用超声提取,0.22μm微孔滤膜过滤,其次采用4000转/min,离心10min后0.22μm微孔滤膜过滤,最后采用供试品直接用0.22μm微孔滤膜过滤进样的方式,结果表明前面两种处理方法和最后一种方法测得结果基本一致,最终选用供试品0.22μm微孔滤膜过滤后直接进样的最简便方式。
本发明没有直接采用现有技术的方法,如以下文献中的方法:
HPLC同时测定益精丸中梓醇和阿魏酸的含量
高效液相色谱法测定地黄叶中梓醇的含量
RP-HPLC-ELSD同时测定复方益母草胶囊中阿魏酸、盐酸水苏碱、梓醇、麦角甾苷的含量
高效液相色谱法测定神康宁丸中梓醇的含量
双波长HPLC法同时测定益肾衍嗣丸中4种成分的含量
高效液相色谱法测定一贯煎颗粒中梓醇的含量
高效液相色谱法测定不同地区地黄饮片中梓醇含量
固相萃取—高效液相色谱法测定太太口服液中阿魏酸含量以及药典中的方法。
而是对上述现有技术的方法进行了大的改进,主要改进点在于:
1.两个成分紫外吸收波长差异较大,采用不同最大吸收波长,分别对俩个成分进行了定量测定。
2.供试品处理方法简单,没有采用文献报道超声、大孔树脂纯化、旋蒸等复杂的处理方式。
改进后的本发明方法大大提高了检测的准确度、缩短了样品处理的时间,测定结果的重复性获得了很大提高。
在以下几个方面优于现有技术:
1.本发明提供的方法操作简单,样品和对照品不需要复杂处理,直接过滤进样;
2.采用等度洗脱,便能同时去除药酒中其他组分干扰,保证测定结果准确可靠;
3.采用高效液相色谱方法测定主要活性成分的含量,更能控制该产品的质量。
附图说明
图1空白溶液色谱峰(70%甲醇);
图2空白溶液色谱峰(0.1%磷酸)
图3去除当归药材的阴性溶液HPLC色谱图;
图4阿魏酸对照品溶液HPLC色谱图;
图5梓醇对照品溶液HPLC色谱图;
图6本发明实施例健脾壮腰药酒中测定阿魏酸的供试品溶液HPLC色谱图;
图7本发明实施例健脾壮腰药酒中测定梓醇的供试品溶液HPLC色谱图;
具体实施方式
下面结合附图和具体实施方式对本发明内容做进一步解释。
实施例1
一种健脾壮腰药酒中测定阿魏酸含量的方法,精密称取阿魏酸对照品10.21mg置50ml量瓶中,加70%甲醇溶解并稀释至刻度,摇匀,作为阿魏酸对照品贮备液,再精密吸取阿魏酸对照品贮备液1ml,加70%甲醇定容至10ml,过0.22μm的滤膜,取续滤液,作为阿魏酸对照品溶液;吸取药酒3ml,过0.22μm的滤膜,取续滤液,即得供试品溶液,平行配制6份;
本发明供试品溶液中阿魏酸的最佳测定方法为:
色谱柱:Agilent ZORBAX SB-C18(4.6*250mm*5μm);柱温:35℃;进样量:10μl;检测波长:316nm;流速:1ml/min;流动相:乙腈-0.1%磷酸(16:84),阿魏酸应和相邻的色谱峰分离度>1.5;运行时间:50min。
测定:分别吸取阿魏酸对照品溶液及供试品溶液各10μl,注入液相色谱仪,测定,即得。
下表为健脾壮腰药酒中阿魏酸含量测定结果。
实施例2
一种健脾壮腰药酒中测定梓醇含量的方法,精密称取梓醇对照品10.83mg置10ml量瓶中,加0.1%磷酸溶解并稀释至刻度,摇匀,过0.22μm的滤膜,取续滤液,即得对照品溶液;吸取药酒适量,过0.22μm的滤膜,取续滤液,即得供试品溶液,平行配制6份;
本发明供试品溶液中梓醇的最佳含量测定方法为:
色谱柱:Agilent ZORBAX SB-C18(4.6*250mm*5μm);柱温:30℃;进样量:10μl;波长:210nm;流速:0.8ml/min;流动相:甲醇-0.1%磷酸(1:99)。
测定:分别精密吸取梓醇对照品溶液及供试品溶液各10μl,注入液相色谱仪,测定,按照外标法计算健脾壮腰药酒中梓醇的含量。
下表为健脾壮腰药酒中梓醇含量测定结果。
本发明的上述实施方案都只能认为是对本发明的说明而不是限制,因此凡是依据本发明的实质技术对以上实施例所作的任何微小色谱条件及其他的改变,均属于本发明技术方案的范围内。
Claims (8)
1.一种健脾壮腰药酒中阿魏酸和梓醇的含量测定方法,其中所述健脾壮腰药酒中阿魏酸的含量测定方法,包括以下步骤:
(1)阿魏酸对照品溶液的制备:取阿魏酸对照品适量,精密称定,加甲醇溶解制成溶液;
(2)供试品溶液的制备:吸取健脾壮腰药酒,过滤,即得;
(3)阴性溶液的制备:按照药酒处方制备不含当归药材的阴性溶液,过滤,即得;
(4)测定:分别精密吸取阴性溶液、阿魏酸对照品溶液及供试品溶液,注入液相色谱仪,得到色谱图,根据色谱图计算阿魏酸的含量。
2.根据权利要求1所述的方法,包括以下步骤:
(1)阿魏酸对照品溶液的制备:取阿魏酸对照品适量,精密称定,加60-800%甲醇溶解制成每1ml约含15-25μg的溶液,过滤,取续滤液,即得;
(2)供试品溶液的制备:吸取健脾壮腰药酒,过滤,取续滤液,即得;
(3)阴性溶液的制备:按照药酒处方制备不含当归药材的阴性溶液,过滤,取续滤液,即得;
(4)测定:分别精密吸取阴性溶液、阿魏酸对照品溶液及供试品溶液各5-20μl,注入液相色谱仪,得到色谱图,根据色谱图计算阿魏酸的含量。
3.根据权利要求1所述的方法,包括以下步骤:
(1)阿魏酸对照品溶液的制备:取阿魏酸对照品适量,精密称定,加70%甲醇溶解制成每1ml约含20μg的溶液,过0.22μm的滤膜,取续滤液,即得;
(2)供试品溶液的制备:吸取健脾壮腰药酒3ml,过0.22μm的滤膜,取续滤液,即得;
(3)阴性溶液的制备:按照药酒处方制备不含当归药材的阴性溶液,过0.22μm的滤膜,取续滤液,即得;
(4)测定:分别精密吸取阴性溶液、阿魏酸对照品溶液及供试品溶液各10μl,注入液相色谱仪,得到色谱图,根据色谱图计算阿魏酸的含量。
4.根据权利要求1所述的方法,其中,所述色谱条件如下:
色谱柱:Agilent ZORBAX SB-C18(4.6*250mm*5μm);柱温:35℃;进样量:10μl;检测波长:316nm;流速:1ml/min;流动相:乙腈-0.1%磷酸(16:84),阿魏酸应和相邻的色谱峰分离度>1.5;运行时间:50min。
5.根据权利要求1所述的方法,其中,健脾壮腰药酒中梓醇含量测定方法,包括以下步骤:
(1)梓醇对照品溶液的制备:取梓醇对照品适量,精密称定,加磷酸制成溶液,即得;
(2)供试品溶液的制备:取健脾壮腰药酒适量,过滤,即得;
(3)阴性溶液的制备:按照药酒处方制备不含地黄药材的阴性溶液,过滤,即得;
(4)测定:测定:分别精密吸取阴性溶液、梓醇对照品溶液及供试品溶液注入液相色谱仪,得到色谱图,根据色谱图计算梓醇的含量。
6.根据权利要求5所述的方法,包括以下步骤:
(1)梓醇对照品溶液的制备:取梓醇对照品适量,精密称定,加0.08-0.12%的磷酸制成每1ml约含0.08-0.12mg的溶液,即得;
(2)供试品溶液的制备:取健脾壮腰药酒适量,过滤,取续滤液,即得;
(3)阴性溶液的制备:按照药酒处方制备不含地黄药材的阴性溶液,过滤,取续滤液,即得;
(4)测定:测定:分别精密吸取阴性溶液、梓醇对照品溶液及供试品溶液各5-20μl,注入液相色谱仪,得到色谱图,根据色谱图计算梓醇的含量。
7.根据权利要求5所述的方法,包括以下步骤:
(1)梓醇对照品溶液的制备:取梓醇对照品适量,精密称定,加0.1%磷酸解制成每1ml约含0.1mg的溶液,即得;
(2)供试品溶液的制备:取健脾壮腰药酒适量,用0.22μm滤膜过滤,取续滤液,即得;
(3)阴性溶液的制备:按照药酒处方制备不含地黄药材的阴性溶液,过0.22μm的滤膜,取续滤液,即得;
(4)测定:测定:分别精密吸取阴性溶液、梓醇对照品溶液及供试品溶液各10μl,注入液相色谱仪,得到色谱图,根据色谱图计算梓醇的含量。
8.根据权利要求5所述的方法,其中所述色谱条件如下:
色谱柱:Agilent ZORBAX SB-C18(4.6*250mm*5μm);柱温:30℃;进样量:10μl;波长:210nm;流速:0.8ml/min;流动相:甲醇-0.1%磷酸(1:99)。
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