正交试验法优选蒙古族药嘎日迪散有效部位提取工艺

目的:优选嘎日迪散有效部位的提取工艺,为后期中试生产提供实验依据。方法:采用非水滴定法测定总生物碱含量;利用UV测定总黄酮含量,检测波长500 nm。以嘎日迪散中总生物碱和总黄酮质量分数为指标,通过正交试验考察乙醇体积分数、溶剂用量、回流时间及提取次数对提取工艺的影响,利用TLC和LC-MS/MS确定提取物中部分生物碱类成分。结果:影响总黄酮提取率的因素主次顺序为回流时间>溶剂用量>乙醇体积分数>提取次数,最佳提取条件组合为加22倍量70%乙醇提取5 h;影响总生物碱提取率的因素主次排序为乙醇体积分数>回流时间>溶剂用量>提取次数,最佳提取条件组合为加26倍量80%乙醇提取4 h;总生物碱和总黄酮质量分数分别为0.139%,0.465%。结论:根据生产实际条件和成本考虑,确定嘎日迪散最佳提取工艺为加22倍量70%乙醇回流提取5 h。野罂粟中主要生物碱类成分为野罂粟碱、黑龙辛甲醚、瑞芙热米定和黑龙辛。

Optimization of Extraction Process of Effective Fraction from Garidi Powders by Orthogonal Test

Objective: To optimize extraction process of effective fraction in Garidi powders and provide experimental evidence for pilot production at later stage. Method: The content of total alkaloids was determined by non-aqueous titration;UV was adopted to determine the content of total flavonoids with detection wavelength at 500 nm.Taking contents of total alkaloids and total flavonoids as indexes,orthogonal test was used to optimize extraction process with ethanol concentration,solid-liquid ratio,extracting time and times as factors,TLC and LC-MS were employed to confirm alkaloids types in extract. Result: Influencing factors acting on yield of total flavonoids was in the order of reflux time > solid-liquid ratio> ethanol concentration > extraction times,optimum extraction conditions of total flavonoids was:extracted 5 h with 22 times the amount of 70% ethanol.Factors acted yield of total alkaloids by ethanol concentration>reflux time>solid-liquid ratio>extraction times,optimum extraction conditions was as followings:extracted 4 h with 26 times the volume of 80% ethanol;mass fractions of total alkaloids and total flavonoids were 0.139% and 0.465%,respectively. Conclusion: According to actual conditions of production and cost,optimum extraction conditions of Garidi powders is as following:reflux extract 5 h with 22 times the volume of 70% ethanol.Main compositions of alkaloids in Papaver nudicaule are nudicauline,amurensinine,reframidine and amurensine.