CN111759873A - 一种前胡超微粉体制备工艺及其质量控制方法 - Google Patents
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Abstract
本发明公开了一种前胡超微粉体制备工艺及其质量控制方法,包括如下步骤:取前胡饮片,采用冷冻干燥干燥至水分≤7.0%;将干燥后的前胡饮片进行超微粉碎,得到粒径35~45μm的前胡超微粉体,包装,即得。本发明制备工艺采用了冷冻干燥和超微粉碎技术相结合,操作环境属于低温(‑20~‑30℃),冷冻干燥能瞬时干燥物料,且避免有效成分的破坏,超微粉碎技术能大大增加药物的比表面积,提高药物中有效成分的溶出速度和溶出率,使药物吸收更容易吸收。本发明采用高效液相色谱法对前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素等多成分进行定量测定,可以全面、客观、准确地控制前胡超微粉体的质量,确保工艺稳定,疗效确切。
Description
技术领域
本发明属于中药粉体饮片加工技术领域,具体涉及一种前胡超微粉体制备工艺及其质量控制方法。
背景技术
前胡在我国药用历史悠久,是一味作用较广的中药材,很多知名化痰止咳类的中成药,如急支糖浆、苏子降气丸等都用到了前胡。近年发现市场上符合药典要求的货源已不多,屡次被提及抽检质量不合格,尤其是含量测定项中白花前胡甲素及白花前胡乙素,因此国家局也在2020年国评品种中将前胡收录,明确提出希望各中药饮片生产企业严格把控产品质量,避免出现不合格现象。
中药超微粉碎技术报道始于90年代中期以后,并均呈逐年增多之势,近两年增长尤快,显示中药超微粉越来越受到重视。这项技术可将植物、动物类原生药材细胞膜或细胞壁打破,使细胞内的药用有效成分直接接触溶媒,利于最大限度吸收利用。因此,为解决当前前胡饮片含量多不合格,质量差异大、药效不保证的情况,结合当前中药超微粉碎技术的应用,前胡尚无相关报道,本发明通过制备前胡超微粉体饮片,提高药物中有效成分的溶出速度和溶出率,使药物吸收更充分,从而提高了药物的生物利用度,以期解决以上问题。
发明内容
为了克服上述现有技术的不足,本发明的首要目的在于提供一种有效物质得到最大保留,且有效物质的溶出速度和溶出率得到明显提高的前胡超微粉体制备工艺。
本发明的再一目的是提供上述前胡超微粉体制备工艺的质量控制方法,该质量控制方法通过建立多指标评测方法,可以全面、客观、准确地控制前胡超微粉体的质量,确保工艺稳定,疗效确切。
本发明是通过以下技术方案实现:
一种前胡超微粉体制备工艺,包括如下步骤:
(1)取前胡饮片,采用冷冻干燥干燥至水分≤7.0%,得到干燥后的前胡饮片;
(2)将干燥后的前胡饮片进行超微粉碎,得到粒径35~45μm的前胡超微粉体,包装,即得。
其中,步骤(1)中,所述冷冻干燥的温度为-20~-30℃,冷冻干燥时间为2~3h,冷冻干燥压力为20~40Pa。
其中,步骤(2)中,所述超微粉碎的设备为振动式药物超微粉碎机,超微粉碎温度为-20~-30℃,超微粉碎时间:20~25min。
其中,步骤(2)中,所述包装是采用聚乙烯塑料袋抽真空/充N2包装。
此外,本发明还公开了上述前胡超微粉体制备工艺的质量控制方法,采用HPLC法同时测定白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分,具体为:
5.1 色谱条件 色谱柱:Thermo accliaim TM120(250mm×4.6mm,5μm);检测器:UV检测器(321nm);以水为流动相A,以乙腈为流动相B,按下表的规定进行梯度洗脱;柱温:30℃;流速:1.0ml/min;
时间/min | 流动相A/% | 流动相B/% |
0~10 | 70 | 30 |
15 | 40 | 60 |
16 | 35 | 65 |
20 | 25 | 75 |
28 | 25 | 75 |
40 | 15 | 85 |
5.2 对照品溶液的制备 精密称取白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素对照品适量,加甲醇制成每1ml各含白花前胡甲素50μg、白花前胡乙素50μg、白花前胡丙素80μg及白花前胡E素60μg的混合对照品溶液;
5.3 供试品溶液的制备 精密称取样品粉末0.5g,置具塞锥形瓶中,精密加入甲醇25ml,称定重量,超声处理(功率250W,频率45kHz)30min,放冷,再称定重量,用甲醇补足减失的重量,摇匀,滤过,取续滤液,即得;
5.4 测定法 取混合对照品溶液,按上述色谱条件,分别吸取不同体积注入高效液相色谱仪进行测定,即得;
本超微粉体按干燥品计算,含白花前胡甲素(C21H22O7)不得少于1.50%,含白花前胡乙素(C24H26O7)不得少于0.45%,含白花前胡丙素(C22H22O8)不得少于1.00%,含白花前胡E素(C24H28O7)不得少于0.60%。
本发明与现有技术相比,具有如下有益效果:
(1)本发明制备工艺采用了冷冻干燥和超微粉碎技术相结合,操作环境属于低温(-20~-30℃),冷冻干燥能瞬时干燥物料,且避免有效成分的破坏,超微粉碎技术能大大增加药物的比表面积,提高药物中有效成分的溶出速度和溶出率,使药物吸收更容易吸收,增加疗效。
(2)本发明采用高效液相色谱法对前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素等多成分进行定量测定,可以全面、客观、准确地控制前胡超微粉体的质量,确保工艺稳定,疗效确切。
附图说明
图1为本发明实施例1的前胡超微粉体的HPLC色谱图。
具体实施方式
下面通过具体实施方式来进一步说明本发明,以下实施例为本发明具体的实施方式,但本发明的实施方式并不受下述实施例的限制。
本发明的实施例及对比例采用的原料均为市场购买。
粒径:采用BT-2001型激光粒度分布仪结合显微镜法进行粒度分布测定,同时以D90值作为反映粒径分布均匀性的指标,并对粉体情况进行描述。
堆密度、休止角:采用BT-100型粉体综合特性测试仪进行测定。
水分、总灰分、酸不溶性灰分、浸出物:按照2015年版《中国药典》规定,分别照前胡项下的水分、总灰分、酸不溶性灰分、浸出物测定方法进行检测并计算含量。
浸膏得率:称取前胡超微粉体饮片5.0g,一次性加入18倍量的沸水浸泡30min,滤过,放冷至室温,备用。精密量取25ml,置已干燥至恒重的蒸发皿中,水浴蒸干后,于105℃干燥3h,置干燥器中冷却30min,精密称定质量,再于105℃干燥1h,同样置干燥器中冷却30min后称定质量,至2次质量的差异不超过0.3mg为止,记录样品的浸膏质量,计算浸膏得率。
实施例1:
一种前胡超微粉体制备工艺,包括如下步骤:
(1)取前胡饮片,采用冷冻干燥干燥至水分≤7.0%,所述冷冻干燥的温度为-25℃,冷冻干燥时间为2.5h,冷冻干燥压力为30Pa,得到干燥后的前胡饮片;
(2)将干燥后的前胡饮片采用振动式药物超微粉碎机进行超微粉碎,超微粉碎温度为-25℃,超微粉碎时间为23min,得到粒径40μm的前胡超微粉体,采用聚乙烯塑料袋抽真空包装,置阴凉干燥处保存,即得前胡超微粉体。测得的前胡超微粉体的休止角、堆密度、水分、总灰分、酸不溶性灰分、浸出物、浸膏得率的结果如表1所示。
制备后,采用高效液相色谱法同时测定前胡超微粉体中白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的含量,具体为:
5.1 色谱条件 色谱柱:Thermo accliaim TM120(250mm×4.6mm,5μm);检测器:UV检测器(321nm);以水为流动相A,以乙腈为流动相B,按下表的规定进行梯度洗脱;柱温:30℃;流速:1.0ml/min;
时间/min | 流动相A/% | 流动相B/% |
0~10 | 70 | 30 |
15 | 40 | 60 |
16 | 35 | 65 |
20 | 25 | 75 |
28 | 25 | 75 |
40 | 15 | 85 |
5.2 对照品溶液的制备 精密称取白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素对照品适量,加甲醇制成每1ml各含白花前胡甲素50μg、白花前胡乙素50μg、白花前胡丙素80μg及白花前胡E素60μg的混合对照品溶液;
5.3 供试品溶液的制备 精密称取样品粉末0.5g,置具塞锥形瓶中,精密加入甲醇25ml,称定重量,超声处理(功率250W,频率45kHz)30min,放冷,再称定重量,用甲醇补足减失的重量,摇匀,滤过,取续滤液,即得;
5.4 测定法 取混合对照品溶液,按上述色谱条件,分别吸取不同体积注入高效液相色谱仪进行测定,测得前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的结果如表2所示。
实施例2:
一种前胡超微粉体制备工艺,包括如下步骤:
(1)取前胡饮片,采用冷冻干燥干燥至水分≤7.0%,所述冷冻干燥的温度为-20℃,冷冻干燥时间为3h,冷冻干燥压力为40Pa,得到干燥后的前胡饮片;
(2)将干燥后的前胡饮片采用振动式药物超微粉碎机进行超微粉碎,超微粉碎温度为-30℃,超微粉碎时间为20min,得到粒径45μm的前胡超微粉体,采用聚乙烯塑料袋充N2包装,置阴凉干燥处保存,即得前胡超微粉体。测得的前胡超微粉体的休止角、堆密度、水分、总灰分、酸不溶性灰分、浸出物、浸膏得率的结果如表1所示。
制备后,采用高效液相色谱法同时测定前胡超微粉体中白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的含量,具体测试方法参考实施例1。测得前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的含量结果如表2所示。
实施例3:
一种前胡超微粉体制备工艺,包括如下步骤:
(1)取前胡饮片,采用冷冻干燥干燥至水分≤7.0%,所述冷冻干燥的温度为-30℃,冷冻干燥时间为2h,冷冻干燥压力为20Pa,得到干燥后的前胡饮片;
(2)将干燥后的前胡饮片采用振动式药物超微粉碎机进行超微粉碎,超微粉碎温度为-20℃,超微粉碎时间为25min,得到粒径35μm的前胡超微粉体,采用聚乙烯塑料袋抽真空包装,置阴凉干燥处保存,即得前胡超微粉体。测得的前胡超微粉体的休止角、堆密度、水分、总灰分、酸不溶性灰分、浸出物、浸膏得率的结果如表1所示。
制备后,采用高效液相色谱法同时测定前胡超微粉体中白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的含量,具体测试方法参考实施例1。测得前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的结果如表2所示。
对比例1:
一种前胡超微粉体制备工艺,包括如下步骤:
步骤(1)取前胡饮片,采用热风循环烘箱/敞开式烘箱60℃干燥至水分≤7.0%,其他步骤均同实施例1,测得的前胡超微粉体的休止角、堆密度、水分、总灰分、酸不溶性灰分、浸出物、浸膏得率的结果如表1所示。
制备后,采用高效液相色谱法同时测定前胡超微粉体中白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的含量,具体测试方法参考实施例1。测得前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的结果如表2所示。
对比例2:
一种前胡超微粉体制备工艺,包括如下步骤:
步骤(2)将干燥后的前胡饮片采用振动式药物超微粉碎机进行超微粉碎,超微粉碎温度为-25℃,超微粉碎时间为15min,得到粒径55μm的前胡超微粉体,其他步骤均同实施例1,测得的前胡超微粉体的休止角、堆密度、水分、总灰分、酸不溶性灰分、浸出物、浸膏得率的结果如表1所示。
制备后,采用高效液相色谱法同时测定前胡超微粉体中白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的含量,具体测试方法参考实施例1。测得前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的结果如表2所示。
对比例3:
一种前胡超微粉体制备工艺,包括如下步骤:
步骤(2)将干燥后的前胡饮片采用振动式药物超微粉碎机进行超微粉碎,超微粉碎温度为-25℃,超微粉碎时间为35min,得到粒径25μm的前胡超微粉体,其他步骤均同实施例1,测得的前胡超微粉体的休止角、堆密度、水分、总灰分、酸不溶性灰分、浸出物、浸膏得率的结果如表1所示。
制备后,采用高效液相色谱法同时测定前胡超微粉体中白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的含量,具体测试方法参考实施例1。测得前胡超微粉体的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的结果如表2所示。
对比例4:
直接取原料前胡饮片;
测得的前胡饮片的水分、总灰分、酸不溶性灰分、浸出物、浸膏得率的结果如表1所示。
采用高效液相色谱法同时测定前胡饮片中白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分,具体测试方法参考实施例1。测得前胡饮片的白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分的结果如表2所示。
表1
休止角/° | 堆密度/g×cm<sup>-3</sup> | 水分/% | 总灰分/% | 酸不溶性灰分/% | 浸出物/% | 浸膏得率/% | |
实施例1 | 43.132 | 0.778 | 5.1 | 4.2 | 1.2 | 39.2 | 60.1 |
实施例2 | 42.784 | 0.767 | 5.1 | 4.1 | 1.3 | 40.1 | 59.5 |
实施例3 | 43.012 | 0.755 | 5.3 | 4.2 | 1.2 | 39.5 | 59.3 |
对比例1 | 45.199 | 0.688 | 6.8 | 5.1 | 1.4 | 32.4 | 55.1 |
对比例2 | 42.021 | 0.737 | 5.9 | 4.9 | 1.3 | 30.5 | 52.0 |
对比例3 | 46.533 | 0.612 | 5.5 | 4.3 | 1.3 | 38.2 | 58.1 |
对比例4 | - | - | 9.2 | 5.5 | 1.5 | 29.1 | 52.1 |
表2
白花前胡甲素/% | 白花前胡乙素/% | 白花前胡丙素/% | 白花前胡E素/% | |
实施例1 | 1.67 | 0.59 | 1.11 | 0.65 |
实施例2 | 1.65 | 0.60 | 1.05 | 0.66 |
实施例3 | 1.59 | 0.51 | 1.02 | 0.65 |
对比例1 | 1.04 | 0.25 | 0.79 | 0.51 |
对比例2 | 1.42 | 0.33 | 0.99 | 0.53 |
对比例3 | 1.34 | 0.41 | 0.92 | 0.52 |
对比例4 | 1.34 | 0.34 | 0.89 | 0.52 |
对实施例1-3及对比例1-4的前胡超微粉体/前胡饮片的质量控制方法进行线性关系、精密度试验、稳定性试验、重复性试验、加样回收率试验,具体如下:
5.1 色谱条件 色谱柱:Thermo accliaim TM120(250mm×4.6mm,5μm);检测器:UV检测器(321nm);以水为流动相A,以乙腈为流动相B,按下表的规定进行梯度洗脱;柱温:30℃;流速:1.0ml/min;
时间/min | 流动相A/% | 流动相B/% |
0~10 | 70 | 30 |
15 | 40 | 60 |
16 | 35 | 65 |
20 | 25 | 75 |
28 | 25 | 75 |
40 | 15 | 85 |
5.2 对照品溶液的制备 精密称取白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素对照品适量,加甲醇制成每1ml各含白花前胡甲素50μg、白花前胡乙素50μg、白花前胡丙素80μg及白花前胡E素60μg的混合对照品溶液;
5.3 供试品溶液的制备 精密称取样品粉末0.5g,置具塞锥形瓶中,精密加入甲醇25ml,称定重量,超声处理(功率250W,频率45kHz)30min,放冷,再称定重量,用甲醇补足减失的重量,摇匀,滤过,取续滤液,即得;
5.4 测定法 取混合对照品溶液,按上述色谱条件,分别吸取不同体积注入高效液相色谱仪进行测定,即得。
一、线性关系 取混合对照品溶液,按上述色谱条件,分别吸取不同体积注入高效液相色谱仪进行测定。以白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素进样量(X)为横坐标、峰面积(Y)为纵坐标,绘制标准曲线,进行线性回归,得到回归方程分别为Y=70.9X-0.0013(R 2 =0.9995)、Y=64.2X-0.4045(R 2 =0.9999)、Y=34.7X+2.3093(R 2 =1.0000)、Y=99.2X-0.2333(R 2 =0.9998),表明白花前胡甲素在0.027~0.543μg、白花前胡乙素在0.033~0.333μg、白花前胡丙素在0.041~0.414μg及白花前胡E素在0.018~0.275μg线性关系良好。
二、精密度试验 取混合对照品溶液,按上述色谱条件,重复进样6次,记录峰面积。结果白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素峰面积RSD分别为0.5%、1.1%、0.9%、0.3%,表明仪器精密度良好。
三、稳定性试验 取同一份供试品溶液分别于配制0、4、8、12、16、20、24h进样分析,记录峰面积,结果白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素峰面积RSD分别为0.8%、1.3%、1.1%、0.2%,表明供试品溶液在24h内稳定。
四、重复性试验 精密称取同一份样品,按供试品溶液的制备方法制备6份供试品溶液,进样分析,计算含量。结果白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素的平均质量分数分别为1.65%、0.60%、1.02%、0.65%,RSD分别为1.3%、1.0%、1.2%、0.8%,表明该方法重复性良好。
五、加样回收率试验 精密称取同一已知含量的样品0.25g,共6份,按1:1加入白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素等对照品适量,按供试品溶液的制备方法制备供试品溶液,按上述色谱条件进样分析,记录峰面积,计算加样回收率,结果白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素的平均回收率分别为100.4%、98.8%、102.2%、101.4%,RSD分别为0.9%、1.2%、1.0%、1.3%,表明该方法准确度符合要求。
Claims (6)
1.一种前胡超微粉体制备工艺,其特征在于,包括如下步骤:
(1)取前胡饮片,采用冷冻干燥干燥至水分≤7.0%,得到干燥后的前胡饮片;
(2)将干燥后的前胡饮片进行超微粉碎,得到粒径35~45μm的前胡超微粉体,包装,即得。
2.根据权利要求1所述的前胡超微粉体制备工艺,其特征在于,步骤(1)中,所述冷冻干燥的温度为-20~-30℃,冷冻干燥时间为2~3h,冷冻干燥压力为20~40Pa。
3.根据权利要求1所述的前胡超微粉体制备工艺,其特征在于,步骤(2)中,所述超微粉碎的设备为振动式药物超微粉碎机,超微粉碎温度为-20~-30℃,超微粉碎时间:20~25min。
4.根据权利要求1所述的前胡超微粉体制备工艺,其特征在于,步骤(2)中,所述包装是采用聚乙烯塑料袋抽真空/充N2包装。
5.如权利要求1-4任一项所述的前胡超微粉体制备工艺的质量控制方法,其特征在于,采用HPLC法同时测定白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素四种成分,具体为:
5.1 色谱条件 色谱柱:Thermo accliaim TM120(250mm×4.6mm,5μm);检测器:UV检测器(321nm);以水为流动相A,以乙腈为流动相B,按下表的规定进行梯度洗脱;柱温:30℃;流速:1.0ml/min;
5.2 对照品溶液的制备 精密称取白花前胡甲素、白花前胡乙素、白花前胡丙素及白花前胡E素对照品适量,加甲醇制成每1ml各含白花前胡甲素50μg、白花前胡乙素50μg、白花前胡丙素80μg及白花前胡E素60μg的混合对照品溶液;
5.3 供试品溶液的制备 精密称取样品粉末0.5g,置具塞锥形瓶中,精密加入甲醇25ml,称定重量,超声处理(功率250W,频率45kHz)30min,放冷,再称定重量,用甲醇补足减失的重量,摇匀,滤过,取续滤液,即得;
5.4 测定法 取混合对照品溶液,按上述色谱条件,分别吸取不同体积注入高效液相色谱仪进行测定,即得;
本超微粉体按干燥品计算,含白花前胡甲素(C21H22O7)不得少于1.50%,含白花前胡乙素(C24H26O7)不得少于0.45%,含白花前胡丙素(C22H22O8)不得少于1.00%,含白花前胡E素(C24H28O7)不得少于0.60%。
6.根据权利要求5所述的前胡超微粉体制备工艺的质量控制方法,其特征在于,还包括对所述前胡超微粉体进行包括粉体休止角、堆密度、水分、总灰分、酸不溶性灰分、浸出物、浸膏得率七项性能指标的测定。
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