ABSTRACT
A quantitative analytical method based on HPLC coupled with the charged aerosol detector (CAD) for quantitative analysis of multi-components with a single marker (QAMS) was established for simultaneous determinations of astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅳ, calycosin-7-O-β-D-glucoside, formononetin and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan in Astragalus membranaceus. The separation was performed on an Agilent SB-C18 (150 mm×4.6 mm, 3.5 μm), with gradient elution using the mobile phase consisting of 0.05% formic acid solution and 0.05% formic acid acetonitrile at the flow rate of 1.0 mL·min-1. The column temperature was 35 ℃, and the injection volume was 20 μL. For CAD, the drift tube temperature was at 50 ℃. The contents of six components in A. membranaceus were determined by both external standard method (ESM) and QAMS, and then were compared. The results showed that chromatographic peaks were separated well and the linear ranges of astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅳ, calycosin-7-glucoside, formononetin and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan were 0.113-2.250 mg·mL-1, 0.012-0.240 mg·mL-1, 0.004-0.080 mg·mL-1, 0.065-1.300 mg·mL-1, 0.005-0.100 mg·mL-1 and 0.007-0.150 mg·mL-1, respectively. The content ranges of astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅳ, calycosin-7-glucoside, formononetin and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan were 0.306-0.922 mg·g-1, 0.053-0.183 mg·g-1, 0.015-0.092 mg·g-1, 0.069-0.823 mg·g-1, 0-0.098 mg·g-1 and 0.020-0.107 mg·g-1 in 20 batches of A. membranaceus, respectively. Using astragaloside Ⅱ as an internal reference, the relative correlation factors of astragaloside Ⅰ, astragaloside Ⅳ, calycosin-7-O-β-D-glucoside, formononetin, and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan were calculated as 0.561, 0.835, 0.299, 0.796, and 0.799, respectively. The results were compared with those obtained by the external standard method to verify the feasibility, rationality and repeatability of QAMS method, and there was no significant difference in assay results between the two methods. In conclusion, the QAMS method is accurate and feasible, and could be used to determine the contents such as astragaloside Ⅰ, astragaloside Ⅱ, astragaloside Ⅳ, calycosin-7-glucoside, formononetin and 7,2'-dihydroxy-3',4'-dimethoxyisoflavan, and it can be used for quality control of A. membranaceus.
ABSTRACT
Objective: To establish a new method for the quantitative analysis of multi-components by single-marker (QAMS) to simultaneous determine six naphthoquinone components in Arnebia euchroma. Methods: The chromatographic peaks of the main naphthoquinone components in A. euchroma were identified by high resolution LC-MS. The acetyl Shikonin was used as internal marker to calculate the relative correlation factors (RCF) of deoxyshikonin, isobutyrylshikonin, β-acetoxyisovalerate shikonin, and β,β'-dimethylacryloyl shikonin by HPLC, and examine the durability and reproducibility of the RCF. The external standard method and QAMS were compared to determine the six components in A. euchroma. Results: The repeatability of RCF was good. The results calculated with QAMS were consistent with the results by the external standard method. Conclusion: The QAMS method for simultaneously measuring the content of six components is accurate and reliable to evaluate the quality of A. euchroma.
ABSTRACT
Objective: To establish a method for the quantitative analysis of multi-components by single marker (QAMS)to determine the content of rutin,linarin,luteolin and apigenin in Herba Cirsii. Methods: Rutin was selected as the internal reference substance,the relative correction factors(RCF)of the other 3 components were established re- spectively,and then the content of each component was calculated according to respective RCF. At the same time,the external standard method was used to determine the content of all four components in Herba Cirsii,the differences be- tween calculated values and measured values were compared,and the method validation was performed. Results: No significant difference was observed between the calculated values and measured ones according to the results from ten batches of Herba Cirsii samples. Conclusion: The validated QAMS method is proved to be of good precision,reproduc- ibility,and reliability which is suitable and feasible for the quality control of Herba Cirsii
ABSTRACT
A quantitative analytical method for multi-components with a single-marker (QAMS) was established for simultaneous determination of neochlorogenic acid, chlorogenic acid, caffeic acid, cryptochlorogenic acid, 1,3-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid in Artemisia capillaris Thunb standard decoction. The separation was performed on a Waters CORTECS T3 column (2.1 mm × 100 mm, 2.7 μm), with the mobile phase consisting of 0.05% phosphate acid solution-acetonitrile for gradient elution. The column temperature was 30 ℃, and flow rate was 0.5 mL·min-1. Using chlorogenic acid as an internal reference, the relative correlation factors of neochlorogenic acid, caffeic acid, cryptochlorogenic acid, 1,3-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid were calculated following UHPLC, as 0.928 0, 0.546 2, 1.099 8, 0.872 1, 1.086 8, 0.739 2, 1.056 6, respectively. The results were compared with those obtained by the external standard method to verify the feasibility, rationality and repeatability of QAMS method. There was no significant difference in assay results between QAMS and the external standard method. In conclusion, the QAMS method is accurate and feasible, and could be used to determine the content such as neochlorogenic acid, caffeic acid, cryptochlorogenic acid, 1,3-dicaffeoylquinic acid, 3,4-dicaffeoylquinic acid, 3,5-dicaffeoylquinic acid and 4,5-dicaffeoylquinic acid in Artemisia capillaris Thunb standard decoction.
ABSTRACT
Objective To establish a quantitative analysis of multi-component with a single-marker (QAMS) method for the quality control of Wuzi Yanzong Pills (WYP). Methods Six main effective components (schisandrin, hyperin, quercitrin, kaempferol 3-O-rutinoside, deoxyschizandrin, and γ-schizandrin) of WYP were simultaneously separated on a reversed-phase column (Ultimate LP-C18) with high-resolution of each chromatographic peak by high performance liquid chromatography (HPLC). Schisandrin was selected as the internal reference, and the relative correlation factors (RCFs) of other five components were calculated to achieve QAMS. The ruggedness of RCFs was tested on different instruments and columns. Moreover, results of the QAMS were compared with the external standard method. Results Within a certain linear range, the RCFs of hyperin, quercitrin, kaempferol 3-rutinoside, deoxyschizandrin, and γ-schizandrin were 0.36, 4.86, 0.88, 7.34, and 6.35, respectively. The repeatability was good under different experimental conditions. There were no significant differences between the calculated value and estimated value on QAMS and external standard method. Conclusion The QAMS method can be used to assay the content of six components of WYP simultaneously and control the quality of WYP simplely, reliably, and accurately.
ABSTRACT
Objective To establish a method for the quantitative analysis of multi-component with a single-marker (QAMS) to determine the contents of four rhubarb anthraquinones inShanzha Xiaozhi capsules; To conduct methodology investigation.Methods Emodin was set as the internal reference substance, and the relative correlation factors of aloe emodin, rhein, chrysophanol to emodin were calculated and evaluated. The contents of these four anthraquinones were determined by the external standard method and QAMS, respectively. Rationality, feasibility and repeatability of the QAMS method were verified by comparing the results obtained from the two different methods. Results The QAMS method and HPLC method did not show significant difference in results.Conclusion QAMS method can be used as a quality assessment model for quantity evaluation of anthraquinones inShanzha Xiaozhi Capsules.
ABSTRACT
OBJECTIVE: To develop a method of quantitative analysis of multicomponents by singlemarker (QAMS) for simultaneous determination of six oligosaccharide esters in Polygalae Radix. METHODS: 3, 6'-Disinapoyl sucrose (DISS) was used as the internal reference substance. The relative correlation factors (RCF) of sibiricose A5, sibiricose A6, tenuifoliside B, tenuifoliside A, and tenuifoliside C to DISS were calculated. The contents of the six oligosaccharide esters in 20 different batches of Polygalae Radix were determined by both external standard method and QAMS. The assay results were compared to evaluate the accuracy of QAMS method. RESULTS: The RCF of sibiricose A5, sibiricose A6, tenuifoiside B, tenuifoliside A, and tenuifoiside C to DISS were 1.23, 1.16, 1.56, 1.79, and 0.92, respectively. Under different experimental conditions, the RCF had good reproducibility, and there was no significant difference in the quantitative analysis results between the external standard method and QAMS method. CONCLUSION: The QAMS method is feasible and credible, and can be used for the quality control of oligosaccharide esters in Polygalae Radix.
ABSTRACT
OBJECTIVE: To establish a quality evaluation method, quantitative analysis of multi-components with a single-marker(QAMS), to simultaneously determine the contents of four flavones in Yinhuang preparations. METHODS: Baicalin was used as the internal reference substance. The relative correlation factors(RCF) of wogonoside, baicalein and wogonin to baicalin were calculated and established. The contents of these four flavones were determined by the external standard method and QAMS respectively. The QAMS method was validated through comparison of the results obtained by the two different methods. RESULTS: Within the linear ranges, the values of RCF determined at 274 nm of wogonoside, baicalein and wogonin to baicalin were 1.20, 1.62 and 1.68 respectively. The RCF showed good reproducibility within the range of 1.7%-4.8% for the three studied compounds. The two methods did not show significant difference in assay results. CONCLUSION: The QAMS method is feasible, credible, and can be used to determine multiple flavones in Yinhuang preparations.
ABSTRACT
OBJECTIVE: To study the feasibility of quantitative analysis of multi-components by single-marker (QAMS) in determination of flavones in Shuanghuanglian preparations by comparing the results assayed by QAMS and external standard method (ESM). METHODS: The analysis was performed on a Xtimate™ C18 column (4.6 mm × 250 mm, 5 μm)with methanol and water containing 0.2% phosphoric acid as the mobile phase in gradient elution. The flow rate was set at 1.0 mL · min-1. The UV detector wavelength was 274 nm, and the column temperature was 30°C. RESULTS: Within the linear ranges, the analysis results showed no significant difference between QAMS and ESM. CONCLUSION: The QAMS method is credible and will be a new quality evaluation pattern for the determination of multiple flavones in Shuanghuanglian preparations.