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复方土荆皮酊处方由土荆皮酊(10%)400毫升,苯甲酸120克,水扬酸60克组成.由于传统质量标准中,只对苯甲酸、水杨酸定性,对在处方中起重要作用的土荆皮没有内控指标,故无法检测。为此,我们用薄层层析法对土荆皮进行定性.另外,对传统酸碱滴定法测总酸量的可靠性及可行性进行了验证.1 土荆乙酸薄层定性1.1 土荆乙酸对照品的制备按文献资料法制备.1 kg 土荆皮粗粉苯渗漉液,以5%碳酸氢钠溶液萃取三次,萃取液合并后加盐酸酸化至PH 6左右,滤出析出物,滤液继续酸化至白色沉淀完全析出,滤取沉淀物,用水洗,抽干,以乙醚—石油醚结晶得簇针状土荆酸8~10g。
The compound earthworm peony root prescription is composed of 400 ml of earth ecdysteroids (10%), 120 g of benzoic acid, and 60 g of salicylic acid. Due to the traditional quality standards, only benzoic acid and salicylic acid are used in the prescription. The earthworm skin, which plays an important role, has no internal control index and cannot be detected. For this purpose, we used TLC to characterize the soil bark. In addition, we verified the reliability and feasibility of the total acidity measured by the traditional acid-base titration method. The preparation of the reference substance was prepared according to the literature data method. 1 kg of benzene osmotic liquid of earthworm skin meal was extracted three times with 5% sodium bicarbonate solution, and the extracts were combined and acidified with hydrochloric acid to about pH 6, and the precipitate was filtered out. Continue to acidify until the white precipitate is completely precipitated. The precipitate is collected by filtration, washed with water, sucked dry, and crystallized in ether-petroleum ether to obtain 8-10 g of needle-like garnetic acid.