快速溶剂萃取联合QuEChERS净化法测定通宣理肺丸中盐酸麻黄碱的方法优选

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目的:研究快速溶剂萃取法(ASE)提取结合QuEChERS净化法测定通宣理肺丸中盐酸麻黄碱的可行性,并将该法与中国药典提取方法进行比较。方法:以通宣理肺丸中盐酸麻黄碱的提取率为指标,通过高效液相色谱法测定其含量,用正交试验优化快速溶剂萃取法的提取条件。结果:快速溶剂萃取法最佳提取条件为:用正己烷对样品进行脱脂(提取温度为80℃,静态提取时间为5 min,提取次数为1次,冲洗体积100%)后进行盐酸麻黄碱的提取,提取溶剂为甲醇,提取温度为80℃,静态提取时间为8 min,提取次数为3次,最后用PSA净化剂进行提取液杂质净化。优化后提取时间缩短至40 min,杂质干扰较小,与中国药典方法比较,结果的RSD在5%以内,可控性强。结论:快速溶剂萃取法结合QuEChERS净化法简单、高效、快速,适用于通宣理肺丸中盐酸麻黄碱的测定。 OBJECTIVE: To study the feasibility of rapid solvent extraction (ASE) extraction combined with QuEChERS purification method for the determination of ephedrine hydrochloride in Tongxuanlifei pill, and to compare the extraction method with that of Chinese Pharmacopoeia. Methods: The extraction rate of ephedrine hydrochloride in Tongxuanlifei pill was taken as an index, and the content of ephedrine hydrochloride was determined by HPLC. The extraction conditions were optimized by orthogonal test. Results: The optimum extraction conditions were as follows: the sample was degreased with n-hexane (extraction temperature was 80 ℃, static extraction time was 5 min, extraction times was 1 and volume of washing was 100% Extraction, extraction solvent for methanol, extraction temperature of 80 ℃, static extraction time of 8 min, the number of extraction was 3 times, and finally with the PSA purification agent impurities purification. After optimization, the extraction time was shortened to 40 min with less impurity interference. Compared with the Chinese Pharmacopoeia method, the RSD of the results was within 5% and the controllability was strong. Conclusion: The rapid solvent extraction method combined with QuEChERS purification method is simple, efficient and rapid, suitable for the determination of ephedrine hydrochloride in Tongxuanlifei pill.
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