ABSTRACT
Objective To establish a new method and validate its feasibilities by the simultaneous quantitative assay of four triterpenes in Poria cocos. Methods A new quality evaluation method of multi-components by single marker (QAMS) was established and validated for P. cocos. Pachymic acid (PA), dehydropachymic acid (DPA), dehydrotumulosic acid (DTA), and dehydrotrametenolic acid (DMA) were selected as analytes while pachymic acid was chosen as internal reference substance to evaluate the quality. The relative correction factor (RCF) of pachymic acid to the other three triterpenes were calculated. The method was evaluated by the comparison of quantity between external standard method and QAMS method. Results The contents of four triterpenes in 17 batches of P. cocos from QAMS method were not significantly different from those from external standard method. Conclusion The method with a single marker is accurate and feasible to determine PA, DPA, DTA, and DMA when some authentic standard substance are unavailable.
ABSTRACT
Objective: To establish the UPLC fingerprint of triterpenoids in Guizhi Fuling Capsule (GFC) and give a new method for quality control. Methods: UPLC was used on an Agilent Zorbox Eclipse Plus HD C18 (100 mm × 2.1 mm, 1.8 μm) column with the gradient elution solvent system composed of acetonitrile-0.1% H3PO4 water solution as mobile phase, the flow rate was 0.2 mL/min, the column temperature was 30℃, and the detection wavelength was 210 nm. The common peaks were identified by Q-TOF/MS. Results: The UPLC fingerprints of triterpenoids in GFC were established. Totally 20 common peaks were selected as the fingerprint peaks of GFC, of which a total of 13 mutual peaks (1-7, 10, 12, and 14-17) from Poria, the peaks of number 8 and 11 were from Cinnamomi Ramulus, the peak of number 9 was from Paeoniae Radix Alba and Moutan Cortex, and the peak of number 13 was from Persicae Semen, Paeoniae Radix Alba, Moutan Cortex, and Cinnamomi Ramulus. The similarity among the fingerprint of 10 batches of GFC samples were 0.90. Fifteen chemical components were identified by UPLC-Q-TOF/MS, which were 1-hederagenin, 2-dehydrotumulosic acid, 3-tumulosil acid, 4-polyporenic acid C, 6-3-epidehydrotumulosic acid, 7-poricoic acid D, 9-α-linolenic acid, 10-dehydropachymic acid, 11-oleanolic acid, 12-pachymic acid, 13-linolic acid, 15-methylcis-9-hexadecenoate, 16-palmitic acid, 17-palmitic acid ethyl ester, and 18-daucosterol. Conclusion: The established UPLC fingerprint has desirable precision, reproducibility, and stability, and could be applied to the quality control of GFC.
ABSTRACT
Objective: To establish an HPLC method for the determination of four triterpene constituents (dehydrotumulosic acid, polyporenic acid C, 3-epi-dehydropachymic acid, and dehydropachymic acid) in Guizhi Fuling Capsules (GFC). Methods: Chromatography conditions were Diamonsic C18 column (250 mm × 4.6 mm, 5 μm), system mobile phase was composed of acetonitrile (A)-0.2% HCOOH aqueous solution (C) in a linear gradient elution mode (0-70 min: 50%-85% A; 70-80 min: 85%-100% A; 80-90 min: 100% A), detective wavelength was set at 242 nm, and column temperature was 40℃. Results: The calibration curve was linear within 0.408-2.04 μg/mL (r = 0.999 9), 0.192-0.96 μg/mL (r = 0.999 5), 0.078-0.39 μg/mL (r = 0.999 5), and 0.075 6-0.378 μg/mL (r = 0.999 5) for dehydrotumulosic acid, polyporenic acid C, 3-epi-dehydropachymic acid, and dehydropachymic acid, respectively. The average recoveries were 97.5% (RSD = 1.4%, n = 5), 98.5% (RSD = 1.6%, n = 5), 97.2% (RSD = 1.2%, n = 5), and 102.3% (RSD = 1.8%, n = 5). Six batches of GFC sample were determined, The average contents of dehydrotumulosic acid, polyporenic acid C, 3-epi-dehydropachymic acid, and dehydropachymic acid were 0.070, 0.015, 0.030, and 0.061 mg/capsule, separately. Conclusion: The method is simple, accurate, and can be used as a quality control method for GFC.
ABSTRACT
OBJECTIVE: To establish an analytical method to determine dehydrotumulosic acid, tumulosic acid, polyporenic acid C, 3-epi-dehydrotumulosic acid, dehydropachymic acid and pachymic acid in poria quickly and accurately. METHODS: An UPLC method was established on an HSS T3 Column (2.1 mm × 100 mm, 1.8 μm). The mobile phase consisted of water (containing 0.05% phosphoric acid) and acetonitrile in gradient elution mode, and the detection wavelength was set at 210 nm. RESULTS: The standard curves of dehydrotumulosic acid, tumulosic acid, polyporenic acid C, 3-epi-dehydrotumulosic acid, dehydropachymic acid, and pachymic acid showed good linearity in 5.400-108.0, 2.040-40.80, 5.020-100.4, 2.120-42.40, 5.060-101.2 and 5.100-102.0 μg · mL-1, respectively and the average recoveries were 98.0% with RSD of 2. 9% for dehydrotumulosic acid, 99. 0% with RSD of 2.8% for tumulosic acid, 101.5% with RSD of 2.5% for polyporenic acid C, 97.1% with RSD of 2.7% for 3-epi-dehydrotumulosic acid, 101.5% with RSD of 2.1% for dehydropachymic acid and 99.6% with RSD of 1.1% for pachymic acid, respectively. CONCLUSION: The method is quick, accurate, and can be used to determine multiple triterpenoid acids in Poria simultaneously.