Study On The Preparative Technology And Quality Control Of Semen Nigellae Total Saponins Dropping Pill

The volatile components were analyzed by headspace solid phase microextraction-gas chromatogr aphy- mass spectrometry(HS-SPME-GC/MS).Twelve components were identified from fifteen separ ated peaks, amounting to 94.8% of the total mass fraction. The comprehensive score including ap pearance quality, weight variation of pills and dissolution time was used as criteria for evaluation.Single factor experiment and orthogonal design were used to optimize the preparation of the seme n nigellae total saponins dropping pill. We Studied on appearance quality, dissolution time, weight variation of pills, TLC and content of determination and established the quality standard of the dr opping pill. With appearance quality, weight variation of pills and dissolution score as indexes for evaluation, the single factor experiment and Box-behnken design(BBD) were used to optimize the preparation of the sustained-release dropping pill. Then we established the quality standard of the sustained-release dropping pill. According to the quality standard of semen nigellae total saponins dropping pill, the stability of the dropping pill was investigated by long-term test and acceleration test for three months. The optimized conditions were as follows. The ratio of PEG4000 to PEG6000 was 5:1. The ratio of total saponins to matrix was l:3. The temperature of drug solution was80℃. The coolant was dimethicone(viscosity was 350 mPa·s). The cooling temperature was 5℃.The dropping distance was 10 cm. The dropping speed was 30 drops per minute. The inside and outside diameters of the dropper was 2/3.5mm. The weight in average was 35 mg per pill. The co ntent of total saponins was 18.1% and it was equivalent to 6.3 mg per pill. The content of semen nigellae saponin A was 14.7% and it was equivalent to 5.1 mg per pill. The results of appearanc e quality, weight variation of pills and TLC were conformed to the standard of the Chinese Pharm aeopoeia. The optimized conditions of the sustained-release dropping pill were as follows. The cont ent of stearic acid in matrix was 40%. The content of semen nigellae total saponins was 30%. Th e temperature of drug solution was 85℃. The coolant was dimethicone which viscosity was 100mPa·s. The cooling temperature was 20℃. The dropping distance was 10 cm. The dropping speed was 30 drops per minute. The inside and outside diameters of the dropper was 2/3.5mm. The we ight in average of the sustained-release dropping pill was 37 mg per pill. The content of total sap onins in the sustained-release dropping pill was 21.4%, and it was equivalent to 7.9 mg per pill.The content of semen nigellae saponin A was 14.6% and it was equivalent to 5.4 mg per pill. No significant changes in individual parameters were found in the long-term test and acceleration test for three months.We prepared the semen nigellae total saponins dropping pill and the sustained- r elease dropping pill and established the quality standards for the two dropping pills. Then we inve stigated the stability of the dropping pill by long-term test and acceleration test for three months.All of these provided the reliable basis for developing drug.