CN111537459A - 一种苦黄颗粒的质量检测方法 - Google Patents
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Abstract
本发明公开了一种苦黄颗粒的质量检测方法,该方法包括:供试品溶液的制备、对照品溶液的制备,标准曲线的制备和供试品溶液的测定。本发明提供的苦黄颗粒的质量检测方法,通过大量实验筛选出最佳的供试品溶液的制备方法,然后采用操作简便的紫外分光光度法检测蒽醌类成分的含量。本发明提供的检测方法,准确度高、稳定性好、重复性好。
Description
技术领域
本发明涉及一种中药制剂的质量检测方法,具体涉及一种苦黄颗粒的质量检测方法。
背景技术
苦黄颗粒由茵陈、柴胡、大青叶、大黄、苦参制成,具有清热利湿,疏肝退黄。用于因湿热内蕴引起的黄疸型病毒性肝炎患者的退黄的作用。其中主要药味大黄含有蒽醌类有效成分。
本发明利用操作简便的紫外发光光度法,建立一种可以测定苦黄颗粒中的蒽醌类成分含量的方法,该方法操作简便,检测效率高,可为更好地监控苦黄颗粒的质量和临床有效性提供依据。
发明内容
发明目的:本发明为了解决现有技术的不足,提供一种精密度高、重复性和稳定性好,操作简便,检测效率高的苦黄颗粒的质量检测方法,从而更有效的保证苦黄颗粒的的质量。
技术方案:为了实现上述目的,本发明采取的技术方案为:
一种苦黄颗粒的质量检测方法,该方法包括以下步骤:
(1)对照品溶液的制备
取经干燥至恒重的1.8-二羟基蒽醌对照品适量,精密称定,加三氯甲烷制成1.8-二羟基蒽醌的对照品溶液,即得;
(2)供试品溶液的制备
取苦黄颗粒,加乙醇超声提取,过滤,得提取液,精密量取提取,加入冰醋酸和盐酸的混合酸和石油醚,置水浴中加热回流提取,放冷,分取石油醚液,再用石油醚同法提取3次,至石油醚层近无色,分取石油醚层,合并石油醚提取液,回收石油醚至干,残渣加混合碱溶液溶解,置水浴中回流,放冷,移至量瓶中,用混合碱溶液洗涤容器,洗液并入量瓶中,加混合碱溶液至刻度,摇匀,避光放置,用双层滤纸滤过,弃去初滤液,取续滤液,得供试品溶液;
(3)标准曲线的制备
精密吸取步骤(1)的对照品溶液0.0,1.0,2.0,3.0和4.0ml,分别置10ml量瓶中,置水浴中挥去三氯甲烷,放冷,加混合碱溶液至刻度,摇匀,避光放置,照紫外-可见分光光度法试验,在525nm波长处测定吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线;
(4)供试品溶液的测定
取步骤(2)的供试品溶液,在525nm的波长处测定吸光度,然后根据步骤(3)的标准曲线读出供试品溶液中1.8-二羟基蒽醌的浓度,与1.125相乘,计算,即得。
作为优选方案,以上所述的一种苦黄颗粒的质量检测方法,该方法包括以下步骤:
(1)对照品溶液的制备
取经105℃干燥至恒重的1.8-二羟基蒽醌对照品适量,精密称定,加三氯甲烷制成每1ml含50μg的1.8-二羟基蒽醌对照品溶液,即得;
(2)供试品溶液的制备
取苦黄颗粒,加乙醇超声提取,过滤,得提取液,精密量取提取液5ml,加体积比为5:1的冰醋酸和盐酸的混合酸2ml和石油醚50ml,置水浴中加热回流提取1小时,放冷,分取石油醚液,再用50ml、30ml、30ml的石油醚同法提取3次,每次约20分钟,至石油醚层近无色,分取石油醚层,合并石油醚提取液,回收石油醚至干,残渣加混合碱溶液15ml溶解,置水浴中回流30分钟,放冷,移至50ml量瓶中,用混合碱溶液洗涤容器,洗液并入量瓶中,加混合碱溶液至刻度,摇匀,避光放置1小时,用双层滤纸滤过,弃去初滤液,取续滤液,得供试品溶液;
(3)标准曲线的制备
精密吸取步骤(1)的对照品溶液0.0,1.0,2.0,3.0和4.0ml,分别置10ml量瓶中,置水浴中挥去三氯甲烷,放冷,加混合碱溶液至刻度,摇匀,避光放置1小时,照紫外-可见分光光度法试验,在525nm波长处测定吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线;
(4)供试品溶液的测定
取步骤(2)的供试品溶液,在525nm的波长处测定吸光度,然后根据步骤(3)的标准曲线读出供试品溶液中1.8-二羟基蒽醌的浓度,与1.125相乘,计算,即得。
作为优选方案,以上所述的苦黄颗粒的质量检测方法,步骤(2)和步骤(3)的混合碱溶液的制备方法为取氢氧化钠25g,加适量的水溶解,放冷,加浓氨试液45ml,用水稀释至1000ml,混匀。
有益效果:本发明提供的苦黄颗粒的质量检测方法相比现有技术具有以下优点:
本发明提供的苦黄颗粒的质量检测方法,通过大量实验筛选出最佳的供试品溶液的制备方法,然后采用操作简便的紫外分光光度法检测蒽醌类成分的含量。本发明提供的检测方法,准确度高、稳定性好、重复性好。
具体实施方式
下面结合具体实施例进一步阐明本发明,应理解这些实施例仅用于说明本发明而不用于限制本发明的范围,在阅读了本发明之后,本领域技术人员对本发明的各种等价形式的修改均落于本申请所附权利要求所限定的范围。
实施例1
一种苦黄颗粒的质量检测方法,该方法包括以下步骤:
(1)对照品溶液的制备
取经105℃干燥至恒重的1.8-二羟基蒽醌对照品适量,精密称定,加三氯甲烷制成每1ml含50μg的1.8-二羟基蒽醌对照品溶液,即得;
(2)供试品溶液的制备
取苦黄颗粒,加乙醇超声提取,过滤,得提取液,精密量取提取液5ml,加体积比为5:1的冰醋酸和盐酸的混合酸2ml和石油醚50ml,置水浴中加热回流提取1小时,放冷,分取石油醚液,再用50ml、30ml、30ml的石油醚同法提取3次,每次约20分钟,至石油醚层近无色,分取石油醚层,合并石油醚提取液,回收石油醚至干,残渣加混合碱溶液15ml溶解,置水浴中回流30分钟,放冷,移至50ml量瓶中,用混合碱溶液(取氢氧化钠25g,加适量的水溶解,放冷,加浓氨试液45ml,用水稀释至1000ml,混匀)洗涤容器,洗液并入量瓶中,加混合碱溶液至刻度,摇匀,避光放置1小时,用双层滤纸滤过,弃去初滤液,取续滤液,得供试品溶液;
(3)标准曲线的制备
精密吸取步骤(1)的对照品溶液0.0,1.0,2.0,3.0和4.0ml,分别置10ml量瓶中,置水浴中挥去三氯甲烷,放冷,加混合碱溶液(制备方法为取氢氧化钠25g,加适量的水溶解,放冷,加浓氨试液45ml,用水稀释至1000ml,混匀)至刻度,摇匀,避光放置1小时,照紫外-可见分光光度法试验,在525nm波长处测定吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线;
(4)供试品溶液的测定
取步骤(2)的供试品溶液,在525nm的波长处测定吸光度,然后根据步骤(3)的标准曲线读出供试品溶液中1.8-二羟基蒽醌的浓度,与1.125相乘,计算,苦黄颗粒含大黄总蒽醌以大黄素(C15H10O5)计为0.300 mg/ml。
Claims (3)
1.一种苦黄颗粒的质量检测方法,其特征在于,该方法包括以下步骤:
(1)对照品溶液的制备
取经干燥至恒重的1.8-二羟基蒽醌对照品适量,精密称定,加三氯甲烷制成1.8-二羟基蒽醌的对照品溶液,即得;
(2)供试品溶液的制备
取苦黄颗粒,加乙醇超声提取,过滤,得提取液,精密量取提取,加入冰醋酸和盐酸的混合酸和石油醚,置水浴中加热回流提取,放冷,分取石油醚液,再用石油醚同法提取3次,至石油醚层近无色,分取石油醚层,合并石油醚提取液,回收石油醚至干,残渣加混合碱溶液溶解,置水浴中回流,放冷,移至量瓶中,用混合碱溶液洗涤容器,洗液并入量瓶中,加混合碱溶液至刻度,摇匀,避光放置,用双层滤纸滤过,弃去初滤液,取续滤液,得供试品溶液;
(3)标准曲线的制备
精密吸取步骤(1)的对照品溶液0.0,1.0,2.0,3.0和4.0ml,分别置10ml量瓶中,置水浴中挥去三氯甲烷,放冷,加混合碱溶液至刻度,摇匀,避光放置,照紫外-可见分光光度法试验,在525nm波长处测定吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线;
(4)供试品溶液的测定
取步骤(2)的供试品溶液,在525nm的波长处测定吸光度,然后根据步骤(3)的标准曲线读出供试品溶液中1.8-二羟基蒽醌的浓度,与1.125相乘,计算,即得。
2.根据权利要求1所述的一种苦黄颗粒的质量检测方法,其特征在于,该方法包括以下步骤:
(1)对照品溶液的制备
取经105℃干燥至恒重的1.8-二羟基蒽醌对照品适量,精密称定,加三氯甲烷制成每1ml含50μg的1.8-二羟基蒽醌对照品溶液,即得;
(2)供试品溶液的制备
取苦黄颗粒,加乙醇超声提取,过滤,得提取液,精密量取提取液5ml,加体积比为5:1的冰醋酸和盐酸的混合酸2ml和石油醚50ml,置水浴中加热回流提取1小时,放冷,分取石油醚液,再用50ml、30ml、30ml的石油醚同法提取3次,每次约20分钟,至石油醚层近无色,分取石油醚层,合并石油醚提取液,回收石油醚至干,残渣加混合碱溶液15ml溶解,置水浴中回流30分钟,放冷,移至50ml量瓶中,用混合碱溶液洗涤容器,洗液并入量瓶中,加混合碱溶液至刻度,摇匀,避光放置1小时,用双层滤纸滤过,弃去初滤液,取续滤液,得供试品溶液;
(3)标准曲线的制备
精密吸取步骤(1)的对照品溶液0.0,1.0,2.0,3.0和4.0ml,分别置10ml量瓶中,置水浴中挥去三氯甲烷,放冷,加混合碱溶液至刻度,摇匀,避光放置1小时,照紫外-可见分光光度法试验,在525nm波长处测定吸光度,以吸光度为纵坐标,浓度为横坐标,绘制标准曲线;
(4)供试品溶液的测定
取步骤(2)的供试品溶液,在525nm的波长处测定吸光度,然后根据步骤(3)的标准曲线读出供试品溶液中1.8-二羟基蒽醌的浓度,与1.125相乘,计算,即得。
3.根据权利要求1或2所述的苦黄颗粒的质量检测方法,其特征在于,步骤(2)和步骤(3)的混合碱溶液的制备方法为取氢氧化钠25g,加适量的水溶解,放冷,加浓氨试液45ml,用水稀释至1000ml,混匀。
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