ABSTRACT
OBJECT IVE To provide reference for the improvement of the quality standard for Niushanggui capsules. METHODS Based on the previous quality standard ，thin-layer chromatography （TLC）identification methods were established for Angelicae dahurica and Anemarrhenae asphodeloides . High performance liquid chromatography （HPLC）method was established to determine the contents of 5 components simultaneously ，such as mangiferin ，prim-O-glucosylcimifugin，naringin，neohesperidin and 5-O-methylvisammioside. The limits were confirmed. RESULTS TLC chromatogram of Niushanggui capsules showed the same color spots in the same position as the corresponding （mixed）substance control or reference medicinal material of A. dahuricae and A. asphodeloides ，while the negative samples had no interference. The linear range of mangiferin ，prim-O-glucosylcimifugin， naringin，neohesperidin and 5-O-methylvisammioside were 7.98-127.63，6.74-107.84，53.06-848.96，39.31-628.90，13.54-216.62 μg/mL，respectively（all r＝0.999 9）. RSDs of precision ，stability（24 h）and repeatability tests were all no more than 1.20％（n＝ 6）. The average recoveries were 95.00％，105.16％，97.16％，101.00％ and 104.97％（RSD≤1.50％，n＝6）. In 4 batches of samples，the average contents of the above 5 components were 0.842，0.696，6.951，5.755 and 1.106 mg/g respectively ；the limits of A. asphodeloides ，Saposhnikovia divaricata and Citrus aurantium were based on the contents of mangiferin ，the total content of prim-O-glucosylcimmifugin and 5-O-methylvisammioside，naringin and neohesperidin ，which would not be less than 0.42，0.90 and 6.36 mg/grain，respectively. CONCLUSIONS TLC identification methods of A. dahurica and A. asphodeloides and the content determination methods of 5 components as mangiferin in Niushanggui capsules are established in this study ，and the limits of A. asphodeloides ，S. divaricata and C. aurantium are confirmed.
ABSTRACT
Objective: To improve the quality standard for Qiangli Pipa distillate formula. Methods: The chemical reactions for i-dentification in the old standard were deleted. TLC methods were established to identify Papaveris pericarpium, Eriobotryae folium and Platycodonis radix. The contents of morphine and codeine phosphate from Papaveris pericarpium were determined by HPLC. The chro-matographic conditions for morphine content determination were as follows: an Inertsil ODS-3 chromatographic column (250 mm × 4. 6 mm, 5 μ m ) was used, the mobile phase was acetonitrile-the mixture of 0. 01 mol·L-1sodium heptane sulfonate and 0. 02 mol ·L-1potassium dihydrogen phosphate with equal amount (10% phosphoric acid was used to adjust pH to 2. 8) ( 13: 87 ), the detec-tion wavelength was 220 nm ,the column temperature was 30 ℃, and the flow rate was 1. 0 ml·min-1. The chromatographic condi-tions for codeine phosphate content determination were as follows : an Inertsil ODS-3 chromatographic column (250 mm×4. 6 mm, 5 μ m ) was used, the mobile phase was acetonitrile-the mixture of 0. 01 mol·L-1sodium heptane sulfonate and 0. 02 mol·L-1s potas-sium dihydrogen phosphate with equal amount (10% phosphoric acid was used to adjust pH to 2. 8) ( 15: 85 ), the detection wave-length was 220 nm, the column temperature was 30 ℃, and the flow rate was 1. 0 ml·min-1. Results: TLC had obvious characteris-tics with clear and well-separated spots. Morphine showed a good linear relationship within the range of 3. 14-62. 8 μg·ml-1( r=1. 000 0) with the average recovery of 96. 69% (RSD=2. 41% , n=9). Codeine phosphate showed a good linear relationship within the range of 3. 52-87. 94 μg·ml-1(r=1. 000 0) with the average recovery of 95. 68% (RSD=2. 64% , n=9). Conclusion: The quality standard for Qiangli Pipa distillate formula is improved. The methods are easy-operated and accurate with good specificity, which are suitable for the quality control of Qiangli Pipa distillate formula.