感冒清热颗粒工艺规程

3.5
3.1
2.9
3.5
2.6
3.3
R2
0.6
0.9
表 3 验证试验结果
批号
进风温度 (℃ ) 喷雾速度 (ml/min) 装袋合格率 (%)
装量差异 (%)
制粒周期 (h)
溶化性
1205111
105~110
3.0
99.4
2.0
12.5
好
1205141
105~110
3.0
99.6
3.1
13.0
好
1205171
·238·
中国现代药物应用2014年10月第8卷第20期 Chin J Mod Drug Appl, Oct 2014, Vol. 8, No. 20
平 , 提高应急、协调、指挥能力 , 时刻保持清醒头脑面对突 发事件。对于急救药品和器械的管理 , 应做到定人员管理 , 定点放置 , 定量储存 , 定期检查维修保养 , 用后及时消毒灭菌 , 及时补充 , 班班交接 , 发现问题立即解决 , 确保急救药品器械 完好率 100%。④稳定院前急救医护人员队伍 , 加强专业技术 培训 , 拓宽急诊专业领域 , 使急诊科医生业务知识广博并且术 业有专攻 , 面对急危重症患者 , 能够做到科内会诊 , 方便、快 捷 , 为患者赢得宝贵的抢救时机 , 提高院前急救的整体水平。 ⑤面对院前急救的现场人员嘈杂、环境复杂的状况 , 医护人 员要做到临危不乱 , 做事有条不紊 , 医护人员到达现场后 , 迅 速对现场状况进行梳理 , 评估现场及周围环境 , 排除不利于现 场急救的环境因素 , 创造有利于现场急救的局部环境 , 必要 时请公安部门配合 , 维护现场抢救秩序。⑥伤员在转运之前 做好止血、包扎、固定工作 , 搬运伤员时动作轻巧 , 协调一致 , 遇脊椎损伤的伤员必须 3 人以上搬运 , 保持脊椎的轴线水平 , 搬运过程中应避免震动、扭曲 , 以免增加伤员痛苦甚至加重 损伤。建立有效的静脉通道 , 选择留置套管时开放静脉通道 , 并牢固固定 , 要做到在转运中患者即使躁动、体位改变静脉 留置套管针也不会脱落 , 保障抢救药品及时输注 , 保障转运 过程的安全。转运途中严密观察局部和全身病情变化 , 对失 血性休克的患者 , 尽早建立两条以上静脉通道 , 转运过程中 合理安排患者体位 , 对出血倾向、头部缺血性疾病 ( 如脑梗死 等患者 ), 患者应将头部朝向车辆前进方向的反方向 , 以免由 于车辆行进时加速作用导致患者脑部进一步缺血。呕吐伴神 志不清的患者取侧卧位 , 昏迷患者取去枕平卧位 , 头偏向一 侧 , 防止窒息。对骨折患者妥善固定患肢于功能位置。

0.61%、1.66%。

薄荷脑、胡薄荷酮、紫苏醛的平均回收率分别为99.00%、102.13%、97.46%，RSD分别为：1.81%、1.71%、1.87%。

6.通过验证5批挥发油样品，证明该含量测定方法适合于相应检测要求。

结论：通过本课题的研究，制定了WER法提取感冒清热颗粒挥发油生产新工艺，工艺参数为：药材破碎，按处方比例称量、混合，采用WER法，加7倍水量，浸泡90min，提取3h。

该工艺提取感冒清热颗粒的提油量与传统工艺（SD）比较，在提油量基本一致的情况下，提取时间由5h降低到3h，具有明显的优势。

通过验证实验和放大实验研究，证明该项新工艺稳定性好，具有产业化实施的前景。

研究制定的感冒清热颗粒挥发油中薄荷脑、胡薄荷酮、紫苏醛的GC 含量测定方法，简便快捷，专属性强，精密度高，重复性好，稳定性好，线性关系良好，加样回收率符合要求，实现了挥发油中三种成分的一次性检测。

所建立的三种成分含量测定方法可以用于感冒清热颗粒挥发油的质量控制，对保证产品质量，确保临床疗效具有现实意义。

关键词：感冒清热颗粒；挥发油；提取工艺；含量测定；胡薄荷酮；薄荷脑；紫苏醛；GCStudy on the Extraction and Determination of volatile oil inGanmaoqingre granuleAbstractGanmao Qingre granules composed of 11 herbs, mint,schizonepeta spike,Saposhnikovia divaricata, bupleurum root, perilla leaf, the root of kudzu vine,Platycodon grandiflorum, bitter almond, angelica,corydalis, reed rhizome.It is considered to have a good effect on the cold cold-induced headache, fever, chills, body ache, cough and throat and other symptoms . It is recorded in the "people's Republic of China Pharmacopoeia" 2010 Edition (a).Studies have shown that, the volatile constituents are the main effective part of Ganmaoqingre granules treating cold, anti-inflammatory, antibacterial and antiviral,antipyretic, antitussive effect.The provisions Chinese Pharmacopoeia standards, schizonepeta spike, mint, basil essential oil components need to be extracted.At present, the volatile oil extraction technology of the product is the distillation method, there is the problem oflong extraction time, extraction efficiency is low, and there is no content control.In order to improve the cold heat granules volatile oilextraction technology level and quality level of control.I conducted this study.Objective :1.To study and formulate Ganmao Qingre granules volatile oil extraction process.2.Establish a GC method to determin three active constituents of the volatile oil in Ganmaoqingre granule once , including Menthol, Pulegone and Perillaldehyde .Methods:1.Study on extraction process of volatile oil in Ganmaoqingre granulePut the amount of oil as the evaluation index to optimize the extraction method. By comparison, Jing Jiesui mint,basil leaves three herbs alone to extract volatile oil and mixed extract volatile oil.The amount of oil as the evaluation index to ascertain extraction technology, through the comparison ofdistillation (SD) and distillation distillation coupling (WER)of two kinds of volatile oil extraction process.Through the combination of water, soaking time, extraction time three factors of different levels of study, orthogonal experimental design, with the amount of oil as the evaluation index, preferably with WER process mixture to extract volatile oil.And through experimental verification and amplification experiments, prove that the method is reproducible and process maturity.In the orthogonal test, determination of the content of menthol, pulegone, and perilla aldehyde in volatile oil,evaluation of different process parameters on the effect ofvarious components of essential oil.2.Method for determination of menthol, pulegone, perilla aldehyde in the volatile oil in Ganmaoqingre granulesUsing gas chromatography (GC) method, based on gas chromatography column type, temperature programmed selection of conditions, internal standard, determined to meet the requirements of the chromatographic conditions.Methodological study by specificity test ,precision test,repeatability, stability test, recovery test, the linear range test .By testing five batches of samples, which are proved feasible method for the content determination.Results:1.According to the three kinds of medicine separate extraction oil 6h, according to the prescription ratio calculation of mixed extraction volume of volatile oil, WER method and SD method are2.43mL and 2.12mL; three herbs mixed extraction 6h, WER method and SD method were 2.88 and 2.95mL . Visible, the extraction of volatile oil in Ganmaoqingre granules, by using three kinds of herbs mixed extraction is appropriate, and the WER was better thanSD.2.Orthogonal experimental results show that the extraction of volatile oil, influence factors of WER Technology: extraction time > soaking time > the amount of water, preferably the best extraction process parameter is A3B2C2, which is 7 times of water, soaking 90min, extraction 3h.3.Experiment and enlarged experiments, results showed that the extraction of volatile oil, Ganmao Qingre granules by WER technology, is reproducible, mature technology, has a good industrial prospect of implementation.4. The sample is separated on a column of DM-FFAP（30 m×0.25mm×0.25 μm）, and detected by FID , the carrier gas is N2 , the speed of flow is 1 mL/min; the temperature of injector and detector is 250 ℃；the temperature of column is from 120 ℃and then heating up to 140 ℃by2 ℃/min；and continue heating up to 220 ℃by 15 ℃/min，and keep 5 minutes, the sample size is 1 μL and the split ratio is 20:1. Menthol is calculated according to the number of theoretical plates should not be less than 110,000, menthol, pulegone, respectively perillaldehyde other adjacent peak separation is greater than 1.5.5.Through the study, the content determination method is specific, menthol( in the 34.034~343.04 μg/mL range), pulegone( in the 88.998~889.98μg/mL range), perilla aldehyde(in the 19.2636~192.636 μg/mL range) respectively, there was a good linear relationship. Good precision instrument, RSD of peak area values were: Menthol 0.88%, pulegone0.97% , perillaldehyde 0.97%. The test solution of menthol, pulegone, perilla aldehyde 24h at room temperature is stable. Experimental good reproducibility, menthol, pulegone, perillaldehyde RSD values were 0.74%, 0.61%, 1.66%. The average recovery of menthol and pulegone and perilla aldehyde rate was 99%, 102.13%, 97.46%, RSD respectively: 1.81%, 1.71%, 1.87%.6.Through the verification of the 5 batch of volatile oil samples, proved this method is suitable for the corresponding testing requirements.Conclusion:Through this research, developed a new extraction technology of volatile oil in Ganmao Qingre granules by WER.Process parameters are as follows: first crushing herbs, then according to the proportion of prescriptions to weighing, mixing, using the method of WER, adding 7 times water, soak 90min, extraction 3H.In the new process(WER) and the traditional process (SD)comparison,Basically the same in the oil amount, extraction time is decreased from 5h to 3h, have obvious advantages.The GC method this research establishment, determination the contents of menthol and pulegone and perilla aldehyde in volatile oil of Ganmaoqingre granules.Simple and quick, specific, high precision, reproducibility, good stability, good linearity, recoveries qualified.The three components in the volatile oil can pass through a sample detected.Can be used for quality control of volatile oil of cold heat particles, to ensure product quality to ensure that the clinical efficacy of practical significanceKey words:Ganmaoqingre granule ,V olatile oil , Extraction ,Determination , Menthol , Pulegone , Perillaldehyde ,GC .中英文对照缩略词表中文名称英文名称英文缩写气相色谱法Gas Chromatography GC提取-共沸精馏耦合工艺Water extractioncoupling rectification WER水蒸气蒸馏法Steam distillation SD感冒清热颗粒挥发油成分的提取工艺及含量测定方法研究引言感冒清热颗粒处方源于清代沈金鳌《杂病源流犀烛》所载荆防败毒散加减化裁而成，由荆芥穗、薄荷、防风、柴胡、紫苏叶、葛根、桔梗、苦杏仁、白芷、苦地丁、芦根11味药材组成，具有疏风散寒,解表清热的功能,用于风寒感冒、头痛发热、恶寒身痛、鼻流清涕、咳嗽咽干的治疗[1]，现收载于《中国药典》2010版（一部）。

《感冒清热颗粒挥发油成分的提取工艺及含量测定方法研究》篇一一、引言感冒清热颗粒是一种广泛应用于中医药治疗感冒的常见药物，其主要功效为清热解毒、散风驱寒。

而其中的挥发油成分，具有显著的药理活性，对感冒的治疗效果起到关键作用。

因此，本文旨在研究感冒清热颗粒中挥发油成分的提取工艺及含量测定方法，以期为提高药物疗效、保证药品质量提供科学依据。

二、材料与方法1. 材料感冒清热颗粒原料药材、无水乙醇、石油醚等。

2. 仪器旋转蒸发器、超声波清洗器、高效液相色谱仪等。

3. 提取工艺（1）粉碎原料药材，使其粒度适中；（2）采用超声波辅助提取法，将粉碎后的药材与无水乙醇混合，进行提取；（3）将提取液进行旋转蒸发，得到挥发油成分。

4. 含量测定方法采用高效液相色谱法对挥发油成分进行含量测定。

三、挥发油成分的提取工艺研究1. 提取条件优化通过改变提取时间、温度、乙醇浓度等条件，对提取工艺进行优化。

采用正交试验法，以挥发油得率为评价指标，确定最佳提取条件。

2. 提取工艺验证在最佳提取条件下，对不同批次、不同产地的感冒清热颗粒原料药材进行提取，验证提取工艺的稳定性和可靠性。

四、含量测定方法研究1. 色谱条件优化通过改变流动相比例、柱温等条件，对高效液相色谱法进行优化，以提高挥发油成分的分离度和测定准确性。

2. 方法学考察（1）标准曲线绘制：将已知浓度的挥发油标准品进行HPLC 测定，绘制标准曲线；（2）精密度试验：对同一浓度的样品进行多次测定，考察方法的精密度；（3）稳定性试验：对样品在不同时间点进行测定，考察样品的稳定性；（4）回收率试验：采用加样回收法，考察方法的准确度。

3. 实际样品测定对提取得到的挥发油成分进行HPLC测定，计算其含量，并与其他方法进行比较，验证本方法的可行性和准确性。

五、结果与讨论1. 提取工艺结果通过正交试验，确定最佳提取条件为：提取时间XX小时，温度XX℃，乙醇浓度XX%。

在此条件下，挥发油得率较高，且各批次、各产地原料药材的提取结果稳定可靠。

正交实验法优选感冒清热颗粒的制备工艺程建峰;刘琳娜;唐永红;王宏涛;杨鹏【摘要】Objective To optimize the preparation procedure of Ganmaoqingre Granules. Methods The volatile oil was extracted by steam-distillation method and included withβ-cyclodextrin ( β-CD). Orthogonal experiment was introduced to optimize the conditions of decoction and volatile oil inclusion, with kakonein transferring ratio as a marker to evaluate the decoction conditions. Results The optimum extraction conditions were as follows:the crude drug which contains volatile oil was extracted with 10 times a-mount of water for 6 hours to collect the volatile oil. The optimal inclusion conditions selected by the orthogonal design were as fol-lows;the ratio of volatile oil to β-CD was 1 : 6,the inclusion time was 1 h and the temperature of inclusion was 40 °C. The optimized conditions for decoction were 2 times (1. 5 h/time) by water with 8 times amount of water. Conclusion This optimized preparation procedure for Ganmaoqingre Granules is stable and feasible.%目的研究感冒清热颗粒的制备工艺.方法采取水蒸气蒸馏法提取挥发油,正交实验设计确定挥发油β-环糊精(β-CD)包合的最佳工艺,以葛根素转移率为指标,优选提取工艺.结果挥发油提取条件为:加10倍量水提取6 h;环糊精最佳包合工艺为:油与β-CD比例为1∶6,恒温40 ℃搅拌包合1 h;煎煮最佳工艺为:加8倍水,煎煮2次,每次1.5 h.结论感冒清热颗粒的制备工艺稳定、可行.【期刊名称】《西北药学杂志》【年(卷),期】2011(026)006【总页数】3页(P451-452,457)【关键词】感冒清热颗粒;正交设计;制备工艺【作者】程建峰;刘琳娜;唐永红;王宏涛;杨鹏【作者单位】第四军医大学唐都医院药剂科,陕西,西安,710038;第四军医大学唐都医院药剂科,陕西,西安,710038;西安澜泰药业有限公司,陕西,西安,710021;西安澜泰药业有限公司,陕西,西安,710021;第四军医大学唐都医院药剂科,陕西,西安,710038【正文语种】中文【中图分类】R944感冒清热颗粒由荆芥穗、薄荷、防风、柴胡、紫苏叶、葛根、桔梗、苦杏仁、白芷、苦地丁、芦根组成，具有疏风散寒、解表清热作用，临床上常用于治疗风寒感冒、头痛发热、恶寒身痛、咳嗽咽干等症。