养阴清肺丸质量分析

Quality analysis on Yangyin Qingfei Pills

目的通过对养阴清肺丸114批样品进行标准检验及7项探索性研究检验,对该品种的质量及标准状况作出总体分析及评价。方法标准检验依据《中国药典》2005年版增补本,其中包括显微鉴别、TLC及HPLC检验。探索性研究检验采用灰分测定法测定成方制剂中总灰分;建立白芍的显微鉴别方法以监测白芍药材未经去皮、炮制不规范等质量问题;增加了玄参的TLC鉴别;运用GC-MS、GC法进行薄荷等挥发性药材的特征图谱测定;建立HPLC法测定制剂中的芍药苷以研究不同企业所用白芍原料的差异;采用HPLC法测定辅料蜂蜜中的有害成分5-羟甲基糠醛(5-HMF);运用加速试验考察药包材的密闭性。结果 26.5%的样品总灰分严重超标;白芍的显微鉴别结果表明20%的生产企业使用炮制不规范的白芍饮片;玄参的TLC都可以检出,但斑点颜色深浅差别较大;近50%的样品缺失薄荷药材的特征峰;芍药苷质量分数最高值约为最低值的4倍,说明不同企业所用药材原料差异较大;由于没有炼蜜的法定限量标准,导致各生产企业使用炼蜜的质量差别极大,5-HMF严重超标,最高达到6mg/g,是未加工蜂蜜国家限量标准(0.04mg/g)的150倍;加速试验结果表明"塑料球壳"与"铝塑板"这两种包装材料的密封性较好。结论各生产企业养阴清肺丸的质量参差不齐,一些企业在原料、辅料、生产工艺及包装材料方面存在着不同程度的问题。按现行质量标准检验合格率97.4%,依据探索性研究方法检验合格率为45.6%,结果表明探索性研究增加了标准的专属性、可控性及安全性,为进一步修订药品标准、控制药品质量提供参考。

Objective There were 114 samples of Yangyin Qingfei Pills analyzed according to the quality standard, seven additional researches on the sample were carried out, and the global quality control and standard condition of this variety were analyzed and evaluated. Methods The standard inspection was based on Chinese Pharmacopoeia （2005）, supplement edition, including microscopic identification, TLC, and HPLC methods. The exploratory research inspection was carried out by using the method of ash determination for analyzing the total ash of preparations. The microscopic identification on Paeoniae Radix Alba was developed for monitoring its quality problems with no-peeled or processed in a non-standard way. TLC identification with Scrophulariae Radix was carried out. The characteristic chromatograms of volatile herbs, such as Menthae Herba, were determined using GC-MS and GC methods. An HPLC method was estabilished for the quantitative determination of Paeonone Radix Alba in preparations to study the differences of raw materials used by different enterprises. The excessive content of a harmful composition in excipients honey, 5-hydroxyl methyl furfural （5-HMF）, was determined by HPLC. Accelerated testing was applied for the impermeability examination of medicine packaging. Results The total ash of 26.5% in the samples exceeded the limited standard badly. Microscopic results of Paeoniae Radix Alba showed that 20% of the enterprises prepared the decoction pieces of Paeoniae Radix Alba by the non-standard processing. All the TLC of Scrophulariae Radix could be detected, while there were great differences in spot colourity among different samples. The samples in nearly 50% did not have the characteristic peak like Menthae Herba. The highest content ofpaeoniflorin was about four times as much as the lowest one, which suggested enterprises used materials in different qualities. Without statutory limit for refined honey, the enterprises used refined honey in various qualities. 5-HMF content exceeded seriously the limited standard up to a maximum of 6 mg/g, which was 150 times the amount of national limits （0.04 mg/g） for unrefined honey. Accelerated testing results showed that the packaging material “plastic spherical shell” and “alumimum-plastic plate”were good at sealing. Conclusion Experimentalresults show that the quality of this drug in each enterprise is uneven. For some enterprises, there have been different problems in raw materials, auxiliary materials, production process, and packing materials. Qualified sample rate is 97.4% according to the current standard of quality inspection. Qualified sample rate is 45.6% based on exploratory research testing method. The results of the test indicate that exploratory research could increase the specificity, controllability, and safety of the standard. It would provide the reference for further revising the drug standard and monitoring the drug quality.