Simultaneous determination of four anthraquinones in Polygonum multiflorum by QAMS / 中国中药杂志

A simple, specific and selective quantitative analysis of multi-components by single marker(QAMS) method for simultaneous determination of anthraquinones and anthraquinone glycosides in Polygonum multiflorum was developed. Four main anthraquinones and its glycosides, emodin, emodin-8-O-β-D-glucoside, physcion and physcion-8-O-β-D-glucoside were selected as analytes to evaluate the quality of P. multiflorum. Emodin was used as the internal standard, and the relative correction factors(RCFs) between emodin and the other three anthraquinones were calculated. Comparison of the contents of the four components in 30 batches of P. multiflorum from different regions and 12 batches decoction pieces from different manufacturers by QAMS and external standard method(ESM) showed that there was no significant difference between QAMS and ESM for quantification of the four main components by using relative error results, and the QAMS method was accurate and reliable, and had a good repeatability. In addition, compared with the results calculated by the difference method between total anthraquinone and free anthraquinone in the content determination of P. multiflorum in Chinese Pharmacopoeia, the results of direct determination combined anthraquinone by QAMS were very close to that by measured the external standard method. Therefore, simultaneous quantification of four main anthraquinones by using QAMS is suitable to evaluate the quality of P. multiflorum. Then the optimized assay method of the combined anthraquinone contents showed simple and feasible, which could be replaced and improved the quantification method of the combined anthraquinone in the current Chinese Pharmacopeia.

Applicability Study on QAMS for Multi-component Content Determination of Lonicerae Japonicae Caulis / 中国中医药信息杂志

Objective To establish a QAMS method for content determination of six compositions (chlorogenic acid, caffeic acid, cryptochlorogenin acid, isochlorogenic acid A, isochlorogenic acid C and loganin) from Lonicerae Japonicae Caulis; To verify the feasibility and applicability of this method in quality control of Lonicerae Japonicae Caulis. Methods Chlorogenic acid was set as internal reference substance. The HPLC analysis was performed on a Waters Symmetry C18 column (4.6 mm × 250 mm, 5 μm) with a mobile phase consisted of acetonitrile and 0.4% phosphoric acid solution in gradient elution manner at a flow rate of 1 mL/min. The column temperature was maintained at 35 ℃, and the detection wavelength was set at 327 nm for chlorogenic acid, caffeic acid, cryptochlorogenin acid, isochlorogenic acid A, isochlorogenic acid C and 236 nm for loganin. Results The relative correction factors of caffeic acid, cryptochlorogenin acid, isochlorogenic acid A, isochlorogenic acid C and loganin were established; there was no obvious difference between calculated value of QAMS and measured value of external standard method. Conclusion The quality control mode of QAMS can be used for multi-index synchronization quality evaluation of the six compositions from Lonicerae Japonicae Caulis.

Determination of Nine Aconitum Alkaloids in Xiaohuoluo Pills with Quantitative Analysis of Multi-compo-nents by Single Marker / 中国药师

Objective:To develop a method of quantitative analysis of multi-components by single marker( QAMS) for nine kinds of alkaloids in Xiaohuoluo pills. Methods: An HPLC-QTOF-MS method with an Agilent ZORBAX Extend-C18 RRHT(2. 1 mm × 50 mm,1. 8 μm) column was applied. The flow rate was 0. 21 ml·min-1 . The column temperature was 30 ℃. The mobile phase was methanol (A)-water (B;containing 0. 1％ formic acid and 2. 5 mmol·L-1 ammonium acetate) with gradient elution. The aconitine was used as the internal standard, and the relative correction factor ( RCFs) of hypaconitine, mesaconitine, benzoylaconine, benzoyl-hypaconine, benzoylmesaconine, aconine, hypaconine and mesaconine was respectively established, and the reproducibility inspection on the RCF was performed. The contents of the other 8 kinds of aconitum alkaloids were calculated according to the RCF. At the same time, an external standard method ( ESM) was performed for the content determination of the nine alkaloids. The results of the two methods were compared. The feasibility and accuracy of the QAMS method were verified. Results:Within a certain range,the RCF of hypacontine,mesacontine, benzoylaconine, benzoylhypaconine, benzoyl mesaconine, aconine, hypaconine and mesaconine to aconitine was 1. 736,1. 979,1. 0471,0. 9242,1. 2901,1. 3078,1. 2859,and 1. 0948,respectively. The QAMS method was established for determi-ning alkaloids. There were no significant differences between the results of the QAMS method and those of the external standard method ( ESM) . Conclusion:With the validation of methodology, the method established in our study can be used for the content determina-tion of aconitine, hypaconitine, mesaconitine, benzoylaconine, benzoylhypaconine, benzoylmesaconine, aconine, hypaconine and mesaconine in xiaohuoluo pills.

Comparison of Simultaneous Determination of Alkaloids in Bile Processed Coptidis Rhizoma by QAMS and External Standard Method / 中国中医药信息杂志

Objective To establish QAMS method to determine the contents of three alkaloids in bile processed Coptidis Rhizoma; To compare the results of QAMS with those from external standard method; To prove the feasibility of QAMS.Methods An HPLC method was developed. Berberine hydrochloride was selected as the internal reference substance. 2 relative correction factors (RCF) of berberine hydrochloride to palmatine hydrochloride and to jatrorrhizine hydrochloride were established. Obtained RCFs were used to conduct content calculation (calculated value) to complete QAMS method. At the same time, the contents (measured value) of the three components were also determined by external standard method. Calculated value and measured value were compared.Results The analysis results showed that there was no significant difference between the calculated values and the measured values of the three alkaloids in 10 batches of bile processed Coptidis Rhizoma.Conclusion The QAMS method can be applied in the determination of alkaloids in bile processed Coptidis Rhizoma.

A quantitative method using one marker for assay of multi-components in Xianling Gubao Capsule / 中草药

Objective: To investigate the positioning based on the relative retention time of fingerprinting and to establish a new quality evaluation method for traditional Chinese medicine preparations, using one chemical reference substance to calcutate multi- components simultaneously. Methods: Employed icariin as the maker component, icariin relative correction factors (RCF) of epimedin C to icariin, asperosaponin VI to icariin, psoralen to icariin and angelicin to icariin were ealeatated in the chromatographic conditions for determination of the four components in Xianling Gubao Capsule (XGC). The contents of icariin were determined by external standard method, and those of epimedin C, asperosaponin VI, psoralen and angelicin were calculated by icariin and their RCF. The accuracy of the new method was evaluated by comparing the relative retention times and calculating the content which using different brands columns for determination. Results: The analysis methods were established,the linearity was good when sample volume was in the range of at 8.2—328.0 ng for icariine(r = 0.999 5), 0.055 6—2.224 μg for epimedin C (r = 0.999 6), 0.144 1—5.764 μg for asperosaponin VI (r = 0.999 6), 5.4—215.2 ng (r = 0.998 0) for psoralen, 6.6—265.6 ng (r = 0.998 5) for angelicin. The average recoveries of asperosaponin VI, psoralen and psoralen were 97.59%, 98.58%, 98.11%, 97.86%, 98.22%, respectively. The RSDs of recovery were all less than 2.0%; There has been no significant difference between the calculated contents and the determined contents, according to the angle cosine value. Conclusion: The method can control the components without providing epimedin C, asperosaponin VI, psoralen, and angelicin reference. The method is not only save reference substance and medicine resources, but also suitable quality evaluation pattern for TCM preparation. This new method made fingerprinting more meaningful in TCM quality control.

Determination of six alkaloids in crude and processed Coptidis Rhizoma with quantitative analysis of multi-components by single marker / 中草药

Objective: To establish a quantitative analysis of multi-components by single marker (QAMS) for the simultaneous determination of six alkaloids in crude and processed Coptidis Rhizoma. Methods: An HPLC method was established to determine the six alkaloids (jatrorrhizine hydrochloride, columbamine hydrochloride, epiberberine hydrochloride, coptisine hydrochloride, palmatine hydrochloride, and berberine hydrochloride) by the external standard method (ESM). With this HPLC method, the berberine hydrochloride was used as the internal standard (IS) to determine five relative correction factors (RCFs) of the five other alkaloids, and their contents in all samples were calculated by their RCFs at the same time. Compared with the content results determined by the ESM and QAMS, the feasibility and accuracy of QAMS method were verified. Results: Within a certain range, the RCFs of jatrorrhizine hydrochloride, columbamine hydrochloride, epiberberine hydrochloride, coptisine hydrochloride, and palmatine hydrochloride to berberine hydrochloride were 1.131, 0.999, 1.011, 1.076, and 1.025, respectively, with the good repeatability in different experimental conditions. There was no significant difference between the QAMS method and ESM method. Conclusion: The QAMS method is feasible and accurate for the simultaneous determination of the six alkaloids in crude and processed Coptidis Rhizoma.

Simultaneous determination of three nucleosides in Cordyceps sinensis by QAMS / 中国药学杂志

OBJECTIVE: To establish a quantitative analysis of multi-components by single-marker (QAMS) method for determination of uridine, guanosine and adenosine in Cordyceps sinensis. METHODS: Adenosine was used as the marker to calculate the relative correction factors (RCF) for uridine and guanosine by using high performance liquid chromatography(HPLC). Both QAMS method and external standard method (ESM) were performed to determine the three kinds of nucleosides in Cordyceps sinensis. RESULTS: There were no significant differences between the two methods. CONCLUSION: The developed QAMS method is feasible to evaluate the quality of Cordyceps sinensis.