ABSTRACT
A quantitative analysis of multi-components by single marker method (QAMS) was established for simultaneous determination of gallic acid, protocatechuic acid, catechin, epicatechin, p-coumaric acid, ferulic acid and phloridzin in Cynomorium songaricum Rupr. The analysis was performed on a ChromCore Polae C18 column (250 mm×4.6 mm, 5 μm) , with a mobile phase consisting of acetonitrile-0.3% phosphoric acid aqueous solution for gradient elution. The volume flow rate, column temperature and sample injection volume were set at 1.0 mL·min-1, 25 ℃, and 40 µL, respectively. The relative correction factors of gallic acid and protocatechuic acid, catechin, epicatechin, p-coumaric acid, ferulic acid and phloridzin were calculated and the durability was also investigated. The contents of these seven compounds in fourteen batches of Cynomorium songaricum Rupr. from different producing areas or batches were determined by external standard method (ESM) and quantitative analysis of multi-components with a single-marker method (QAMS), respectively. SPSS and Origin Pro software were employed for principal components assay, similarity evaluation and cluster analysis. The specificity, precision, repeatability, stability and linear range (R2 > 0.999 0) of the seven components were all good. The average recovery was 96.89%-103.16% and RSD was 0.55%-2.76%. Then gallic acid was chosen as internal reference for calculation the correction factors for the other six components, the average relative correction factors of protocatechuic acid, catechin, epicatechin, p-coumaric acid, ferulic acid and phloridzin were 1.141 5, 0.200 5, 0.208 0, 2.361 9, 1.867 7, 0.204 6, respectively. Student's test results showed that there was no significant difference between the data analyzed by ESM and the data obtained from QAMS method. Through data visualization analysis, the contents of gallic acid, protocatechuic acid, catechin and epicatechin in different samples were significantly different, indicating that these four components might be the main quality markers of Cynomorium songaricum Rupr. for gaving more contributes to the principal components. The cluster analysis showed that samples from Xinjiang and samples from Inner Mongolia were clustered in significantly different categories, meaning that the quality of Cynomorium songaricum Rupr. had great relation with producing areas. The method of QAMS established in this study is a simple, economical and practical method with scientific and applicable charactistics for evaluating the quality of Cynomorium songaricum Rupr. efficiently and scientifically.
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
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 develop a method of quantitative analysis of multi-components by single marker (QAMS) for six active ingredients in Gualoupi injection. Methods: An HPLC method was used with a Waters Sunfire ODS C18column (250 mm×4. 6mm, 2. 5 μm), the mobile phase was methanol(A)-0. 2% glacial acetic acid solution(B) with gradient elution, the flow rate was 1. 0 ml· min-1,the detection wavelength was 254 nm,the column temperature was 30℃ and the injection volume was 20 μl. Using 3, 29-dibenzoyl rarounitriol as a reference, the relative correction factors among karounidiol, vanillic acid, adenosine, quercitrin and cynaro-side were detected by QAMS and their contents were calculated, and the results were compared with those of the external standard method. Results: The differences were not statistically significant between the calculated values of karounidiol, vanillic acid, adeno-sine, quercitrin and cynaroside and those measured by the external standard method (P>0. 05). Conclusion: QAMS can be used for the determination of 6 effective components in Gualoupi injection, and the result is accurate, simple and effective.
ABSTRACT
Objective To establish a quantitative method for the simultaneous measurement of the residual level of three pesticides in Nelumbinis semen by GC-MS/MS. Methods The samples were extracted by acetonitrile and purify by Cleanert TPH column. The samples were then tested by GC-MS/MS. Information on relative retention time and mass charge ratio was used for qualitative analysis. The peak area obtained by secondary ion MS of bifenthrin (181.1/166.1)was used as the reference peak to calculate the relative correction factor for the peak area of fenpropathrin (265.1/210.1) and deltamethrin (252.9/93.0), to establish a method using bifenthrin as the reference substance to determinate there sidual quantity of three pesticides in Nelumbinis semen by GC-MS/MS. Results When the injection quantity of the sample containing bifenthrin,fenpropathrin and deltamethrin in the range of 0.01-0.1 ng , there was a good linear relationship between the injection quantity and peak are a Limitation of quantification (LOQ) of bifenthrin , fenpropathrin and deltamethrin were 4.321×10-4 ng, 3.435×10-4 ng, 8.913×10-3 ng, respectively. The average recovery rates of bifenthrin, fenpropathrin and deltamethrin were 93.5％, 93.5％ and 93.8％, respectively. Conclusions The method of quantitative analysis of multi-components with a single-marker is simple, quick and accurate. It suitable for the detection of residual quantity of bifenthrin, fenpropathrin and deltamethrin in Nelumbinis semen.
ABSTRACT
Objective: This study aimed to simultaneously determine six composition of Panax ginseng by quantitative analysis of multi-components with a single-marker (QAMS) in different paris. Methods: Phenomenex Luna C18 (250 mm × 4.6 mm, 5 μm) was used with mobile phase consisting of acetonitrile-0.1% phosphoric acid for gradient elution at a flow rate of 1.0 mL/min, The column temperature was 25 ℃ and the detection wavelength was 203 nm. Ginsenoside Rb1 was used as reference to establish its relative correction factor of Rg1, Re, Rc, Rb2, Rd, The contents of six components were determined by both external standard method and QAMS. and t test was used to evaluate the feasibility and applicability of QAMS. Results: In a certain linear range, the relative correction factor (RCF) was good, No significant differences were observed between the quantitative results of the two methods. Conclusion: It is feasible and suitable to evaluate the quality of Panax ginseng. It can provide a useful reference to quality control of multi-indexed components in Chinese herbs and traditional Chinese preparations.
ABSTRACT
Objective To establish a combined quality evaluation model of fingerprint and quantitative analysis of multi-components with a single-marker (QAMS) to analyze the total flavonoids from licorice residue by the chemical conversion method; To provide technical support for quality control in production. Methods Total flavonoids of breaking cell wall and enriching were taken as the object of study to establish fingerprint. With liquiritin as internal reference, the relative correction factors of isoliquiritin, glycyrrhizin, isoliquiritigenin and glycyrrhizic acid were established respectively, and the contents were determined. Meanwhile, the calculated values were compared with the measured value by external standard method to verify the practicability and stability of QAMS. Results The HPLC fingerprint of total flavonoids from licorice residue was established. 11 common peaks were identified, and 5 common peaks were identified, and the similarity of the 10 extracts was >0.99; the relative error between the calculated results of QAMS and the measured values of the external standard method was <4%; the RSD of relative correction factor calculated by the multiple concentration method was <2%. Conclusion The method is accurate, reliable, specific, and stable, with good repeatability, which can be used for the quality control of total flavonoids from licorice residue.
ABSTRACT
Objective To establish a quantitative analysis of multi-components with a single-marker (QAMS) method for the determination of nine components in Yiqi Fumai Injection (YFI). Methods Ginsenoside Rb1 was used as internal reference substance. The relative correlation factors (f) of ginsenosides Rg1, Re, Rf, Rc, Ro, Rb2, Rd, and schisandrin were calculated and established by HPLC. The separation was performed on a Diamonsil® C18 column (2) (250 mm × 4.6 mm, 5 μm), with the mobile phase consisting of acetonitrile and 0.05% phosphoric acid water for gradient elution. The column temperature was 30 ℃, and the detection wavelength was set at 203 nm, flow rate was 1 mL/min. The results were compared with those obtained by the external standard method in 25 batches of YFI. Results Ginsenosides Rg1, Re, Rf, Rb1, Rc, Ro, Rb2, Rd, and schisandrin had good relations within the ranges of 0.929-4.644, 0.818-4.089, 0.732-3.660, 1.461-7.305, 0.636-3.181, 0.618-3.092, 0.788-3.941, 0.758-3.789, and 0.178-0.889 μg, respectively. The recovery rates were 97.08%-100.94%. The f values of ginsenosides Rg1, Re, Rf, Rc, Ro, Rb2, Rd, and schisandrin to ginsenoside Rb1 were 1.970, 0.929, 1.196, 0.870, 0.830, 0.786, 0.906, and 12.082. The two methods did not show the significant difference in assay results. Conclusion The QAMS method is feasible and credible, and could be used to determine the multiple components in YFI.
ABSTRACT
Objective To establish a methodological study pattern of quantitative analysis of multi-components by single marker ( QAMS) , and examine its feasibility and technical applicability in the quality control of compound preparation of traditional Chinese medicine-Jinhoujian spray. Methods Gas chromatographic method ( GC) was used and naphthalene served as the internal standard. Menthol was used as the reference substance. The relative correlation factors ( RCF) of 1,8-Cineole, camphor and borneol to menthol were calculated and established to carry out QAMS.The accuracy of this method was confirmed by comparison of internal standard method. Results The reproducibility of relative correction factor was perfect. The two methods did not show significant difference in 10 bathes of samples. Conclusion The QAMS method is feasible, credible, and can be used to determine active ingredients in Jinhoujian spray.
ABSTRACT
Objective: To establish a quantitative analysis of multi-components with a single-marker (QAMS) method for the determination of the nine components in Reduning Injection (RI), comparing with the external standard method, and to evaluate the adaptation and application of QAMS method in the quality control of RI. Methods: Chlorogenic acid, isochlorogenic acid A, and gardenoside were used as the internal reference substances. The relative correlation factors (f) of neochlorogenic acid, cryptochlorogenic acid, and caffeic acid to chlorogenic acid, isochlorogenic acid B and isochlorogenic acid C to isochlorogenic acid A, and secoxyloganin to gardenoside were calculated and established. The results were compared with those obtained by the external standard method. Results: Within the linear ranges, the f values of chlorogenic acid to neochlorogenic acid, cryptochlorogenic acid, and caffeic acid were 0.965, 0.991, and 0.555, respectively; isochlorogenic acid A to isochlorogenic acid B and isochlorogenic acid C were 1.283 and 1.129, respectively; jasminoidin to secoxyloganin was 1.030. The two methods did not show the significant difference in assay results. Conclusion: The QAMS method is feasible and credible, and could be used to determine the multiple components in RI.
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.