| Liuwei’anxiao capsule is composed of 6 kinds of Traditional Chinese Medicine. This paper is about studies on the quality control standard of Liuwei’anxiao capsule. The present study provides methods to determine the index components in Liuwei’anxiao capsules by gas chromatography and high performance liquid chromatography, respectively. The integrated quality assessment of Liuwei’anxiao capsules was developed.Two compounds were isolated from the volatility oils of Inula helenium L., and they were identified as follow by spectral analysis:alantolactone and iso-alantolactone. And eleven compounds were isolated from the roots of Rheum tanguticum Maxin ex Regel. by silica gel, Sephadex LH-20 and Polyacylamine chromatography and they were identified as follow by chemical reactions and spectral analysis:chrysophanol, emodin, physcion, aloe-emodin, rhein, cinnamic acid, gallic acid, catechin, 1-O-galloy-2-O-cinnamoyl-β-D-glucose,β-sitosterol and daucosterol.A GC method was developed to determine the contents of alantolactone and iso-alantolactone in Inula helenium L.. The analysis was performed on PEG-20M capillary column (30 m×0.25 mm×0.25μm) with nitrogen as the carrier gas, and ethyl-p-hydroxybenzoate was used as an internal standard. The liner response range were 0.024-0.24 mg-mL-1 (r= 0.9998),0.029-0.29 mg-mL-1 (r= 0.9996), respectively (n= 6); the average recoveries (n= 9) of alantolactone and iso-alantolactone were 98.3% and 98.0%, respectively. And the method was developed to determine the content of ethyl-p-methoxycinnamate in Kaempferia galanga L. The liner response range was 0.192-1.92 mg-mL-1 (r= 0.9999), the average recovery (n= 9) of ethyl-p-methoxycinnamate was 98.1%. The GC method was developed to determine the contents of alantolactone, iso-alantolactone and ethyl-p-methoxycinnamate in Liuwei’anxiao capsule simultaneously. The liner response range were 0.024-0.240 mg-mL-1 (r= 0.9999), 0.029-0.290 mg-mL"1 (r= 0.9999) and 0.192-1.920 mg-mL-1 (r= 0.9996), respectively (n= 6); the average recoveries (n= 9) of alantolactone, iso-alantolactone and ethyl-p-methoxycinnamate were 98.8%,98.4% and 98.7%(n= 9), with RSD of 1.8%,1.4% and 1.0%, respectively. The method is simple, quick and accurate. It is suitable for quality control of this preparation.An HPLC method was developed to determine the contents of aloe-emodin, rhein, emodin, chrysophanol and physion in Liuwei’anxiao Capsules. The analysis was carried out with a Diamonsil-C18 (4.6 mm×200 mm,5μm) column and a mobile phase of methanol-0.05% phosphoric acid solution, gradient elution. The flow rate was 1.0 mL-min-1 and column temperature was 35℃. The detection wavelength was set at 254 nm. The calibration curve was linear within the range of 1.622-16.22μg·mL-1,0.6960-6.960μg·mL-1,2.448-24.48μg·mL-1, 2.752-27.52μg·mL-1,2.702-27.02μg·mL-1 for aloe emodin, rhein, emodin, chrysophanol and physion, respectively. The average recoveries were 97.8%(RSD= 1.2%, n= 9),99.6%(RSD = 1.5%, n= 9),101.8%(RSD= 1.5%, n= 9),98.7%(RSD= 1.2%, n= 9) and 98.3%(RSD= 1.7%, n=9) for aloe-emodin, rhein, emodin, chrysophanol and physion, respectively. This method is convenient, accurate and reproducible for determination of aloe-emodin, rhein, emodin, chrysophanol and physion in Liuwei’anxiao Capsules.An HPLC method was developed to determine the contents of Gallic acid in Liuwei’anxiao Capsules. The analysis was carried out with a Diamonsil-C18(4.6 mm×200 mm,5μm) column by UV detector at 272 nm with a mobile phase of methanol-0.05% phosphoric acid solution (12:88). The flow rate was 1.0 mL·min-1 and column temperature was 35℃. The calibration curve showed a good linearity within the range of 4.58-45.80μg·mL-1. The average recovery was 99.8% with RSD of 0.8%(n= 9). This method is simple, rapid and accurate for determination of gallic acid in Liuwei’anxiao Capsules. |
PDF Full Text Request