Simultaneous Determination of 4 Components in Shenbai Shuxin Granules by HPLC / 中国药房

OBJECTIVE:To establish a method for simultaneous determination of sodium danshensu,protocatechuic aldehyde,salvianolic acid B and phellodendrine hydrochloride in Shenbai shuxin granules.METHODS:HPLC method was adopted.The separation was performed on Waters sunfire-C18 column with mobile phase consisted of acetonitrile-0.05 ％ trifluoroacetic acid (gradient elution) at the flow rate of 1.0 mL/min.The detection wavelength was set at 288 nm,and the column temperature was 30 ℃.The sample size was 5 μL.RESULTS:The linear ranges of sodium danshensu,protocatechuic aldehyde,salvianolic acid B and phellodendrine hydrochloride were 0.040 01-1.600 46 μg(r=0.999 9),0.013 84-0.553 7 μg(r=0.999 9),0.049 32-1.972 94 μg(r=0.999 6),0.014 46-0.578 6 μg(r=0.999 8).The limits of quantitation were 7.68,2.66,4.74,1.38 ng,and the limits of detection were 1.92,0.66,2.36,0.69 ng,respectively.RSDs of precision,stability and reproducibility tests were all lower than 2％.The recoveries were 98.846％-100.762％ (RSD=0.77％,n=6),96.632％-99.463％ (RSD=0.98％,n=6),98.541％-100.432％ (RSD=0.82 ％,n =6),98.607 ％-101.521％ (RSD =1.11％,n =6),respectively.CONCLUSIONS:The method is simple,accurate and precise.It can be used for 4 components in Shenbai shuxin granules.

Study on Quality Standards forAnshu Liquid / 中国中医药信息杂志

Objective To establish quality standards forAnshu Liquid.Methods Phellodendri Chinensis Cortex and Kochiae Fructus were qualitatively identified by TLC method. The contents of berberine hydrochloride and phellodendrine hydrochloride in the preparation were determined by HPLC method. The chromatographic column was ZORBAX SB-C18 (4.6 mm×250 mm, 5μm); the mobile phase was acetonitrile-0.1% phosphoric acid (0.5% diethylamine) gradient elution; the flow rate was 1.0 mL/min; the detection wavelength was 284 nm.Results Berberine hydrochloride and phellodendrine hydrochloride in Phellodendri Chinensis Cortex and saponin Ic in Kochiae Fructus were detected by TLC method. The linear relationship of berberine hydrochloride in the preparation was Y=23.109X?30.548,r2=0.999 8, RSD=2.97%, showing that the linear range of berberine hydrochloride was 0.050 5– 2.525 0 μg. The linear relationship of phellodendrine hydrochloride in the preparation wasY=10.038X?2.446 6, r2=0.999 9, RSD=1.24%, showing that the linear range of phellodendrine hydrochloride was 0.050 0–2.500 0 μg. Conclusion The method is accurate, rapid, stable and reliable, with good reproducibility, which can be used for the quality control and evaluation ofAnshu Liquid.

Application of quantitative 1H NMR for the calibration of protoberberine alkaloid reference standards.

Quantitative nuclear magnetic resonance spectroscopy (qNMR) has been developed into an important tool in the drug analysis, biomacromolecule detection, and metabolism study. Compared with mass balance method, qNMR method bears some advantages in the calibration of reference standard (RS): it determines the absolute amount of a sample; other chemical compound and its certified reference material (CRM) can be used as internal standard (IS) to obtain the purity of the sample. Protoberberine alkaloids have many biological activities and have been used as reference standards for the control of many herbal drugs. In present study, the qNMR methods were developed for the calibration of berberine hydrochloride, palmatine hydrochloride, tetrahydropalmatine, and phellodendrine hydrochloride with potassium hydrogen phthalate as IS. Method validation was carried out according to the guidelines for the method validation of Chinese Pharmacopoeia. The results of qNMR were compared with those of mass balance method and the differences between the results of two methods were acceptable based on the analysis of estimated measurement uncertainties. Therefore, qNMR is an effective and reliable analysis method for the calibration of RS and can be used as a good complementarity to the mass balance method.