气相指纹图谱在加味藿香正气制剂质量评价中的应用

目的建立气相指纹图谱方法,测定不同厂家的加味藿香正气制剂的气相指纹图谱,探讨加味藿香正气制剂的质量差异。方法采用气相色谱法,以100%聚二甲基硅氧烷为固定相,程序升温,初始温度150℃,保持8 min,以每分钟2℃的速率升温至180℃,保持5 min,再以每分钟2℃的速率升温至220℃;保持10 min,流速:1.0 m L/min;进样口温度280℃;检测器温度280℃;分流进样,分流比10∶1;测定3个不同厂家的加味藿香正气制剂的气相指纹图谱,采用相似度软件进行评价。结果不同剂型的加味藿香正气制剂的指纹图谱存在较大差异。结论该方法可用于加味藿香正气制剂的质量评价。

Applying risk management to analytical methods for the desorbing process of ginkgo diterpene lactone meglumine injection

Analysis errors can occur in the desorbing process of ginkgo diterpene lactone meglumine injection(GDMI) by a conventional analysis method, due to several factors, such as easily crystallized samples, solvent volatility, time-consuming sample pre-processing, fixed method, and offline analysis. Based on risk management, near-infrared(NIR) and mid-infrared(MIR) spectroscopy techniques were introduced to solve the above problems with the advantage of timely analysis and non-destructive nature towards samples. The objective of the present study was to identify the feasibility of using NIR or MIR spectroscopy techniques to increase the analysis accuracy of samples from the desorbing process of GDMI. Quantitative models of NIR and MIR were established based on partial least square method and the performances were calculated. Compared to NIR model, MIR model showed greater accuracy and applicability for the analysis of the GDMI desorbing solutions. The relative errors of the concentrations of Ginkgolide A(GA) and Ginkgolide B(GB) were 2.40% and 2.89%, respectively, which were less than 5.00%. The research demonstrated the potential of the MIR spectroscopy technique for the rapid and non-destructive quantitative analysis of the concentrations of GA and GB.

基于质量源于设计理念优化参蒲盆炎颗粒喷雾干燥工艺

目的基于"质量源于设计"(quality by design,Qb D)理念,采用设计空间法优化参蒲盆炎颗粒喷雾干燥工艺。方法首先将集粉率、水分含量及芍药苷、绿原酸、虎杖苷、丹酚酸B含量6个指标作为关键质量属性(critical quality attribute,CQA),采用Plackett-Burman(P-B)设计实验,通过加权标准偏回归系数筛选出进风温度、进样速率、药液密度为3个关键工艺参数(critical process parameter,CPP);再采用Box-Behnken设计实验,通过逐步回归法建立CQA和CPP间的数学模型。结果方差分析显示模型P值均小于0.05,失拟值均大于0.05,可以较好地描述CQA和CPP之间的关系。最后通过MonteCarlo仿真法计算获得基于概率的设计空间并验证。结论在工艺参数设计空间内操作能够保证参蒲盆炎颗粒喷雾干燥工艺品质稳定,有助于提高批次间质量均一性,为产业化提供数据支撑。

Impact of parameter fluctuations on the performance of ethanol precipitation in production of Re Du Ning Injections, based on HPLC fingerprints and principal component analysis

The present study was designed to determine the relationships between the performance of ethanol precipitation and seven process parameters in the ethanol precipitation process of Re Du Ning Injections,including concentrate density,concentrate temperature,ethanol content,flow rate and stir rate in the addition of ethanol,precipitation time,and precipitation temperature.Under the experimental and simulated production conditions,a series of precipitated resultants were prepared by changing these variables one by one,and then examined by HPLC fingerprint analyses.Different from the traditional evaluation model based on single or a few constituents,the fingerprint data of every parameter fluctuation test was processed with Principal Component Analysis(PCA)to comprehensively assess the performance of ethanol precipitation.Our results showed that concentrate density,ethanol content,and precipitation time were the most important parameters that influence the recovery of active compounds in precipitation resultants.The present study would provide some reference for pharmaceutical scientists engaged in research on pharmaceutical process optimization and help pharmaceutical enterprises adapt a scientific and reasonable cost-effective approach to ensure the batch-to-batch quality consistency of the final products.