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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 To evaluate the quality and standard status of 114 samples of Yangyin Qingfei Pill by standard test and 7 exploratory research tests. Method standard test based on “Chinese Pharmacopoeia” 2005 edition supplement, including microscopic identification, TLC and HPLC test. Exploratory research test using ash determination of total ash in the preparation of prescriptions; the establishment of white peony root microscopic identification method to monitor peony un-peeled, non-standard processing and other quality problems; increased TLC identification of Scrophulariaceae; use GC-MS, GC method for the determination of the characteristics of volatile compounds such as mint map; HPLC method was established to determine paeoniflorin in the preparations to study the differences of raw materials used in different enterprises; Paeonia byzodinate Methyl furfural (5-HMF); use of accelerated test to examine the tightness of the drug package. The results showed that 26.5% of the samples had serious total ash content. The results of microscopic identification of white peony root indicated that 20% of the producing enterprises used the unprocessed white peony root slices, TLC of Scrophularia ningpoensis could be detected, 50% of the samples were missing the characteristic peaks of peppermint herbs; the highest value of paeoniflorin was about 4 times of the lowest value, which indicated that the raw materials used by different enterprises were quite different. Because there was no statutory limit standard for refining honey, The quality of honey is very different, the 5-HMF is seriously over-standard, up to 6mg / g, which is 150 times of the national limit of unprocessed honey (0.04mg / g); the accelerated test results show that “ Aluminum plate ”The two packaging materials better sealing. Conclusions The quality of Yangyin Qingfei Pills from various manufacturers is uneven. Some enterprises have different degrees of problems in raw materials, auxiliary materials, production technology and packaging materials. According to the current quality standard test pass rate of 97.4%, based on exploratory research methods test pass rate of 45.6%, the results show that the exploratory study increased the standard specificity, controllability and safety, in order to further revision of drug standards, control of drug quality for reference.