基于质量源于设计(QbD)理念的喘贴灵提取工艺研究

Extraction process in Chuantieling (CTL) based on the quality by design (QbD) concept

    摘要
  • 摘要:
    目的基于质量源于设计（QbD）理念设计并优化喘贴灵水提工艺。
    方法采用单因素实验筛选喘贴灵水提最佳实验点，在此基础上，以盐酸麻黄碱转移率、芥子碱硫氰酸盐转移率和浸膏得率为评价指标。选择液料比、提取时间及pH值作为主要考察因素，进行Box-Behnken设计（BBD）。建立关键质量属性（CPPs）与关键工艺参数（CQAs）的数学模型，考察CQAs与CPPs的交互作用，建立喘贴灵提取工艺设计空间并进行优化，保障该工艺的稳定性。使用高效液相色谱法（HPLC）分析喘贴灵提取液中主要有效成分。
    结果通过单因素筛选实验，选择液料比为8∶1，提取时间为90 min，pH值为4以及提取次数3次为最佳实验点进行后续实验。BBD方差分析结果显示回归模型的P值小于0. 05，且失拟值大于0. 01，表明所建模型具有较好的预测能力。喘贴灵水提工艺CPPs的操作空间结合实际生产的情况，最佳提取工艺为加水倍数9倍，提取时间72 min，pH值 4.5。HPLC结果显示喘贴灵提取液中含盐酸麻黄碱、芥子碱硫氰酸盐、延胡索乙素、甲基丁香酚、桂皮醛和6-姜酚的峰面积分别占喘贴灵提取液总峰面积的0.94%、14.32%、0.78%、31.23%、0.34%和0.44%。
    结论基于QbD理念建立的喘贴灵水提工艺设计空间，有利于实际生产操作，保障其工艺稳定性。

     

    Abstract:
    ObjectiveThis study aimed to design and optimize the water extraction process for Chuantieling (喘贴灵, CTL) based on the concept of quality by design (QbD).
    MethodsThe single-factor experiments were used to select the best experimental points of CTL water extraction. On this basis, the transfer rate of ephedrine hydrochloride and sinapine thiocyanate, and the yield of the extract were evaluated as the evaluation indicators. The liquid-solid ratio, extraction time, and pH value were selected as the main factors to carry out the Box-Behnken design (BBD). A mathematical model of the critical process parameters (CPPs) and critical quality attributes (CQAs) was established, the interaction between CQAs and CPPs was examined, and the CTL extraction process design space was established and optimized, which guaranteed the stability of the process. The high performance liquid chromatography (HPLC) was used to analyze the main active compounds in the CTL extract.
    ResultsThrough single-factor experiments, the best experimental parameters were found to be a liquid-solid ratio of 8∶1, extraction time of 90 min, pH value of 4, and extraction times of three. The experimental variance analysis results of the BBD showed that the P value of the regression model was less than 0.05, and the lack-of-fit value was greater than 0.01, indicating that the constructed model had good predictive ability. The operating space of the CPPs of the CTL water extraction process was combined with the actual production situation. In the production situation, the best extraction process was nine times of water addition, 72 min of extraction time, and 4.5 of pH value. The HPLC results showed that the peak areas of ephedrine hydrochloride, sinapine thiocyanate, tetrahydropalmatine, methyl eugenol, cinnamaldehyde, and 6-gingerol in the CTL extract accounted for 0.94%, 14.32%, 0.78%, 31.23%, 0.34%, and 0.44% of the total peak area, respectively.
    ConclusionThe water extraction process design space of CTL based on QbD was conducive to actual production operations, ensuring the stability of the process.

     

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