ABSTRACT
Objective To establish an HPLC method for simultaneous determination of loganin, chiratin, secoxyloganin, rosmarinic acid and calceolarioside B in Shuangxiangpaishi granules. Method HPLC colunmn was Alltima C18 column (4.6 mm×250 mm, 5 μm); mobile phase consisted of acetonitrile-methanol (1: 3) (A) -0.1% phosphate acid solution (B) with gradient elution; the column temperature was 35°C; the flow rate was 1.0 ml/min; all the injection volume was 20 μl; loganin, chiratin and secoxyloganin were detected at 240 nm, rosmarinic acid and calceolarioside B were detected at 330nm. Results The above mentioned five main ingredients had linearity in the given concentration range at 5.91-118.20 μg/ml (r=0.9995), 4.10-82.00 μg/ml (r=0.9991), 8.13-162.60 μg/ml (r=0.9993), 12.57-251.40 μg/ml (r=0.9998), 4.95-99.00μg/ml (r=0.9997), respectively. The average recoveries (n=6) and RSD were 96.88 (1.31), 99.09 (1.47%), 98.29 (1.59), 98.82 (1.42) and 97.51 (0.86), respectively. Conclusion This dual-wavelength HPLC method could simultaneously determine the contents of the five ingredients in Shuangxiangpaishi granules and can be used to evaluate their quality. The method is simple, accurate, sensitive and repeatable. It could be used as an efficient strategy for systematic quality evaluation of Shuangxiangpaishi granules.
ABSTRACT
Objective To establish a method of quality control for compound Cornu cervi degelatinatum tablets. Methods Thin layer chromatography ( TLC ) was used for qualitative identification of Lonicerae Japonicae Caulis and Pyrola Herba in the preparations. High performance liquid chromatography was used to determine the content of loganin and chiratin in Lonicerae Japonicae Caulis and monotropein in Pyrola Herba. Results The TLC spots were clear and specific in the qualitative identification.HPLC determined the content. In the concentration range, monotropein, loganin and chiratin had a good linear relationship with peak area (r>0.999).The mean recovery was 97.2%, 98.4% and 96.0%;RSD was 1.4%, 0.8% and 0.8%. Conclusion The present study employs TLC for quality control and HPLC for quantity control. The methods are simple and accurate, have good reproducibility, and can effectively control the quality of compound Cornu cervi degelatinatum tablets.
ABSTRACT
OBJECTIVE: To establish a method for the quality control of Lonicerae Japonicae Flos by multi-components quantitative fingerprint. METHODS: Chlorogenic acid was selected as the marker of ingredients to establish the HPLC fingerprint and as the internal reference standard to determine the contents of other eight components(neochlorogenic acid, cryptochlorogenic acid, chiratin, rutin, galuteolin, isochlorogenic acid B, isochlorogenic acid A and isochlorogenic acid C) according to the relative correction factor of quantitative analysis of multi-components by single marker(QAMS) by slope correction method. At the same time, the nine components were determined by external standard method. The accuracy and feasibility of QAMS were evaluated by comparison of the results between external standard method and QAMS. RESULTS: The fingerprint of Lonicerae Japonicae Flos was established, 21 common peaks were identified in all the tested samples, nine of which were verified, the similarities of 20 batches of Lonicerae Japonicae Flos samples were in the range of 0.959-0.997, and there was no significant difference between the quantitative test results of nine ingredients in 20 batches by the QAMS method and external standard method. CONCLUSION: The method of multi-marker components quantitative fingerprint is feasible and accurate for the quality control of Lonicerae Japonicae Flos, and it might be a new quality evaluation pattern for Traditional Chinese medicine.
ABSTRACT
Objective: To establish a method for the determination of loganic acid, chiratin, and loganin in Dipsaci Radix and improve the quality evaluation by analyzing Dipsaci Radix from different habitats. Methods: The analysis was performed on Venusil MP C18 column (250 mm×4.6 mm, 5 μm) with mobile phase consisting of 0.1% H3PO4-acetonitrile for gradient elution: 0-10 min, 8%-9% B; 10-30 min, 9%-11% B; 30-35 min, 11%-100% B. The flow rate was 1 mL/min and the column temperature was 25℃. Results: The results showed that loganic acid, chiratin, and loganin were well separated with the good linearity in 18.4-368.2, 2.02-40.4, and 17.5-349.6 μg/mL, respectively. The average recoveries of the three iridoid glycosides were 99.34%, 99.19%, and 101.61%. Conclusion: Loganic acid, chiratin, and loganin are the main iridoid glycosides in Dipsaci Radix. The method can easily be applied to the content determination of loganic acid, chiratin, and loganin in Dipsaci Radix quickly. The content ranges of loganic acid, chiratin, and loganin are 20.4-186.8, 26.4-177.7, and 1.9-13.2 mg/g, respectively, and the sum of the three iridoid glycosides shows no significant differences in various Dipsaci Radix from different habitats, and proposes to evaluate the quality of Dipsaci Radix.