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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.
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This study establishes a quantitative analysis of multi-components by single marker (QAMS) method for the simultaneous determination of gallic acid, sodium danshensu, protocatechuic acid, protocatechuic aldehyde, vanillin, rosmarinic acid, salvianolic acid B, eugenol, cryptotanshinone and tanshinone IIA in Guanxinshutong capsules (Bambusae Concretio Silicea, Salvia miltiorrhiza, clove, borneol, Bambusae Concretio Silicea) by HPLC. Sample was loaded onto an Agilent C18 (ZORBAX Extend-RP C18, 250 mm × 4.6 mm, 5 µm) column and eluted with methanol-0.4% aqueous formic acid solution as a flow phase gradient, flow speed 1.0 mL·min-1, detection wavelength 280 nm, column temperature 35 ℃ and sample intake of 5 µL. Using protocatechuic acid as the internal reference, a relative correction factor was calculated and the durability was investigated, and the content of 10 components was calculated by QAMS and external standard method (ESM). The results show that the specificity, linear relationship, precision, repeatability, and stability of the 10 components were good. The average recovery was 98.20%-103.47% and RSD was 1.26%-2.84%. The relative positive factors and contents of the other nine components were calculated as gallic acid (0.759, 227.381), sodium tanshinol (3.630, 3.283), protocatechualdehyde (0.185, 0.150), vanillin (0.532, 65.213), rosmarinic acid (4.240, 1.035), salvianolic acid B (3.245, 18.204), eugenol (1.729, 9.265), cryptotanshinone (0.691, 1.449), and tanshinone ⅡA (0.702, 1.939). The results of QAMS were consistent with ESM analysis, and the relative error was between -3% and 3%. This method is stable and reliable, and can be used for the determination of 10 components in Guanxinshutong capsules.
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To establish a quantitative analysis of multi-components by single marker (QAMS) for the determination of Aster souliei Franch., the relative correction factors (fx) of neochlorogenic acid, cryptochlorogenic acid, rutin, isoquercitrin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, quercetin, apigenin and kaempferol were established by ultra-high performance liquid chromatography with chlorogenic acid as internal reference. Meanwhile, the content of each component was determined by the external standard method (ESM) and QAMS, and a linear regression model was established to verify the feasibility and accuracy of the QAMS. Hierarchical clustering analysis (HCA) and orthogonal partial least square discriminate analysis (OPLS-DA) were used to evaluate the quality of 23 batches of A. souliei. The results showed that the repeatability of each fx was good. The average content of neochlorogenic acid, cryptochlorogenic acid, rutin, isoquercitrin, isochlorogenic acid B, isochlorogenic acid A, isochlorogenic acid C, quercetin, apigenin and kaempferol in 23 batches of A. souliei by QAMS was 0.165, 0.234, 6.115, 0.478, 0.484, 3.359, 1.382, 0.210, 0.172, and 0.057 mg·g-1, respectively. The mean content determined by the ESM method was 0.163, 0.235, 6.172, 0.479, 0.483, 3.343, 1.413, 0.207, 0.171, and 0.056 mg·g-1. The results of HCA and OPLS-DA analysis show that 23 batches of A. souliei can be divided into two groups based on caffeic acid content. The content of the first group was between 0.873 to 5.647 mg·g-1, while the second was between 8.524 to 16.705 mg·g-1. This QAMS method can be used to simply and quickly evaluate the quality A. souliei.
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OBJECTIVE：To establish the method for simultaneous determination of 11 active components in Yuhuai tablets ， such as gardoside ，shanzhiside，gardenoside，genipin 1-gentiobioside，geniposide，ziyuglycoside Ⅰ ，ziyuglycoside Ⅱ ，narirutin， naringin，hesperidin and neohesperidin. METHODS ：HPLC-QAMS method was adopted. The determination was performed on Agilent TC-C 18column（250 mm×4.6 mm，5 μm）with mobile phase consisted of acetonitrile （A）-0.1％ phosphoric acid solution （B） （gradient elution ）at the flow rate of 1.0 mL/min. The column temperature was set at 30 ℃. The detection wavelengths were set at 238 nm for gardoside ，shanzhiside，gardenoside，genipin 1-gentiobioside and geniposide ，203 nm for ziyuglycoside Ⅰ and ziyuglycoside Ⅱ，and 283 nm for narirutin ，naringin，hesperidin and neohesperidin. Using geniposide as an internal reference ，the relative correction factors of other 10 components relative to this component were calculated ，and the contents of each component in 10 batches of samples were calculated. The results obtained by HPLC-QAMS method were compared with those obtained by external standard method. RESULTS ：The linear ranges of gardoside ，shanzhiside，gardenoside，genipin 1-gentiobioside，geniposide， ziyuglycoside Ⅰ，ziyuglycoside Ⅱ，narirutin，naringin，hesperidin and neohesperidin were 0.87-43.50，1.99-99.50，4.06-203.00， 7.35-367.50，12.97-648.50，28.98-1 449.00，3.79-189.50，1.57-78.50，18.05-902.50，0.66-33.00 and 14.38-719.00 μg/mL（all r＞0.999 0）. RSDs of precision ，repeatability and stability （24 h）tests were all less than 2％（n＝6）. The average recoveries were 96.90％-100.10％，and RSDs were 0.67％-1.74％（n＝9）. E-mail：289931673@qq.com There was no significant difference in the contents of 10 active components as gardoside between HPLC -QAMS method and external standard method in 10 batches of Yuhuai tablets （P＞0.05）. CONCLUSIONS ：The HPLC-QMAS method established in this study is convenient and accurate. It can be used for the simultaneous determination of gardoside ，shanzhiside，gardenoside，genipin 1-gentiobioside，geniposide，ziyuglycoside Ⅰ，ziyuglycoside Ⅱ，narirutin，naringin，hesperidin and neohesperidin in Yuhuai tablets.
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To establish a quantitative analysis of multi-components by single marker(QAMS) method for five flavonoids in Rhododendron anthopogonoides and verify its feasibility and applicability in the medicinal materials of R. anthopogonoides. With hyperoside as the internal reference, relative correction factors(RCF) of rutin, quercetin, quercitrin and kaempferol were established by high-performance liquid chromatography(HPLC) analysis. RCFs were used to calculate the content of each component, system durability and relative retention time. Simultaneously, QAMS and external standard method(ESM) were used to determine the content of five flavonoids in 12 batches of R. anthopogonoides from different origins. The results were statistically analyzed to verify the accuracy and feasibility. The fingerprints and cluster analysis data of R. anthopogonoides analyzed and discussed differences among the batches. According to the results, the RCFs of rutin, quercetin, quercetin and kaempferol in R. anthopogonoides were 1.242 6, 0.990 5, 0.535 0, and 0.781 3, respectively. The RCFs represented a good reproducibility under different experimental conditions. Besides, there was no significant difference between QAMS and ESM. Besides, the fingerprint and cluster analysis data showed the consistency between the classification and with the origin distribution of the herbs. In conclusion, the QAMS method shows a good stability and accuracy in the quality control of R. anthopogonoides.
Subject(s)
Chromatography, High Pressure Liquid , Drugs, Chinese Herbal , Flavonoids , Medicine, Tibetan Traditional , Reproducibility of Results , RhododendronABSTRACT
Objective::To establish the quality control method for multi-index content determination and fingerprint of salvianolic acids. Method::Agilent ZORBAX SB-C18 (4.6 mm×250 mm, 5μm) column was adopted, with 0.1%formic acid-water as mobile phase A and 0.1%formic acid-acetonitrile as mobile phase B for gradient elution (0-30 min, 20%-21.5%B; 30-35 min, 21.5%-25%B; 35-45 min, 25%-40%B; 45-50 min, 40%-95%B). The column temperature was set at 30 ℃, the flow rate was set at 1 mL·min-1, and the detection wavelength was set at 288 nm. Relative correction factors of caffeic acid, salvianolic acid E, rosmarinic acid, lithosperic acid, salvianolic acid B and salvianolic acid Y were determined by the concentration method. The content of each indicator component of the reference extract of salvianolic acid polyphenolic acid was determined and compared with the results of the monomer reference substance by the external standard method. At the same time, the fingerprint method was established. and the similarity evaluation was carried out on 10 batches of extracts. Result::Caffeic acid, salvianolic acid E, rosmarinic acid, lithospermic acid, salvianolic acid B, and salvianolic acid Y had a good linear relationship within the respective detection mass concentration ranges (r>0.999 9). The injection precision RSD was 0.1%-1.2%, the reproducible RSD was 1.2%-1.6%, and the recovery of the six components was 82.03%-98.68%. The stability of each component in the sample solution was good within 36 h. The relative correction factors for each indicator component were determined to be caffeic acid (2.92), salvianolic acid E (1.10), rosmarinic acid (1.61), lithosperic acid (1.07), salvianolic acid B (1.00), salvianolic acid Y (0.83). The effects of different methods, concentrations, instruments, columns, wavelengths were investigated, and the measured relative correction factors were found to be suitable. The results of the calibration factor method and the monomer standard reference substance method were less different. The HPLC fingerprints of the reference extract of salvianolic acids were established, and five common characteristic peaks were determined. The chromatographic peaks were confirmed according to the reference substance. The similarity of the fingerprints of the 10 batches of extracts was higher, and the quality difference was smaller. Conclusion::The multi-index content determination method and the fingerprint method established in this study are simple, rapid, accurate and reproducible, and can be used for quality control of Salviae miltiorrhizae Radix et Rhizoma polyphenolic acid reference extract.
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Objective::To establish the HPLC fingerprint of carbonized ginger and to determine the contents of zingerone, 6-gingerol, 6-shogaol, 10-gingerol, 8-shogaol and 10-shogaol with quantitative analysis of multi-components by single marker (QAMS). Method::The fingerprint of carbonized ginger was established by HPLC. All samples were analyzed by Waters SymmetryShield™ RP18 column (4.6 mm×250 mm, 5 μm) with gradient elution by acetonitrile(A)-water(B) (0-30 min, 25%-70%A; 30-50 min, 70%-90%A; 50-60 min, 90%A), the flow rate was 1.0 mL·min-1, the detection wavelength was set at 240 nm and the column temperature was 30 ℃. Zingerone, 6-gingerol, 8-gingerol, 6-shogaol, 10-gingerol, 8-shogaol and 10-shogaol was chosen as marker ingredients to establish HPLC fingerprint of carbonized ginger decoction pieces. Taking 6-gingerol as internal reference standard, the contents of zingerone, 6-shogaol, 10-gingerol, 8-shogaol and 10-shogaol were determined at the detection wavelength of 220 nm and 280 nm according to the relative correction factor. Result::The HPLC fingerprint of carbonized ginger was obtained and 10 common peaks were designated, and 7 of them were identified as zingerone, 6-gingerol, 8-gingerol, 6-shogaol, 10-gingerol, 8-shogaol and 10-shogaol, respectively. And there were no significant differences between the quantitative results of external standard method and QAMS. It is suggested that the content limits of carbonized ginger should be not less than 0.020%of zingerone (C11H14O3), 0.050%of 6-gingerol (C17H26O4), 0.120%of 6-shogaol (C17H24O3), 0.080%of 10-gingerol (C21H34O4), 0.030%of 8-shogaol (C19H28O3) and 0.050%of 10-shogaol (C21H32O3) calculated with reference to the dried products, respectively. Conclusion::The developed method is accurate and feasible, which can provide a simple and effective method for the quality control of carbonized ginger.
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To solve the problems of the poor resolution of chromatographic separation,the weak durability of the relative correction factors,and the low accuracy of content determination results in the quantitative analysis of multi-components by single-marker( QAMS) method with andrographolide as the internal reference substance in the existing research of Andrographis Herba,a new QAMS method using dehydroandrographolide as the internal reference substance was established for the first time in this study. This new method can be used to simultaneously determine four diterpene lactones,including andrographolide( A),neoandrographolide( B),14-deoxyandrographolide( C),and dehydroandrographolide( S) through the optimization of chromatographic conditions and systematic investigation of methodology. At the present HPLC chromatographic conditions,four components could be well separated( R > 1. 5),and the methodology validations could satisfy the requirement of quantitative analysis. The relative correction factors( RCFs) of fA/S,fB/S,fC/S were determined as 0. 65,0. 54,0. 78,respectively. The relative standard deviations( RSDs) of their RCFs ranged between 1. 3%-5. 1%,0. 25%-0. 33%,0. 070%-0. 15%,0. 070%-0. 22%,respectively with three brands of HPLC instruments,five brands of C18 column,different flow rates( 0. 9,1. 0,1. 1 m L·min~(-1)),and different column temperatures( 25,30,35 ℃),indicating good durability of the RCFs. The relative retention value( RRV) method was used to locate the chromatographic peak of the components to be determined.The RRVs of rA/S,rB/S,and rC/Swere 0. 44,0. 86,0. 97,respectively. The RSDs of the RRVs ranged between 0. 030%-1. 6% with different HPLC instruments and columns,showing accurate peak location. The present QAMS method and the external standard method( ESM)were both used to determine the contents of four diterpene lactones from Andrographis Herba( 6 batches of medicinal materials and 18 batches of cut crude drugs). The relative errors of the determined content results between two methods were less than 2. 0%. It demonstrated that there was no significant difference in content results between these two methods,indicating good accuracy of the present QAMS method. Therefore,in this study,an accurate and highly durable QAMS method using dehydroandrographolide as the internal reference substance was established for simultaneous determination of four diterpene lactones. This method could be used to effectively control the quality of Andrographis Herba and provide technical basis for the formulation of traditional Chinese medicine industry standard and improvement of the Chinese Pharmacopoeia standard of Andrographis Herba.
Subject(s)
Andrographis , Chromatography, High Pressure Liquid , Diterpenes , Drugs, Chinese Herbal , Quality ControlABSTRACT
Objective: To establish quantitative analysis of multi-components with single marker (QAMS) for determination of 10 phloroglucinol contents in effective fraction of Dryopteris fragrans. Methods: The relative correction factors of nine phloroglucinol (aspidin PB, aspidin AB, flavaspidic acid BB, saroaspidin A, flavaspidic acid PB, disflavapidic acid PB, flavaspidic acid AB, compound VI, and aspidinol B) were determined by HPLC method with the aspidinn BB as the internal standard, which were to calculate the content of each. At the same time, external standard method (ESM) was used to determine the contents of 10 components in effective fraction, and the differences between the two methods were compared to verify the feasibility and accuracy of QAMS method. Results: The relative correction factor (RCF) was good. There was no significant difference between the quantitative results with the two methods in the 12 batches of 10 phloroglucinols. Conclusion: The established QAMS method can be used for quantitative analysis of D. fragrans with aspidinn BB as the internal standard in the absence of reference substances, and provided a reference for the multi-index quality evaluation in effective fraction of D. fragrans.
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Objective: The purpose of this study was to establish a QAMS analytical method for 16 compounds in Psoraleae Fructus, and attempt to evaluate the quality difference among different batches of Psoralen Fructus by chemometrics. Methods: All experiments were performed on three different HPLC instruments. Isopsoralen was used as the internal reference substance to determine the relative correction factors of the other 15 compounds. The robustness and durability of the measured relative correction factors of the 15 compounds were evaluated on different chromatograph instruments and columns; And the measurement result deviation was compared between QAMS method and the external standard method. Results: Under the established chromatographic conditions, the relative correction factors of 15 compounds in Psoraleae Fructus had high accuracy, good durability, and good reproducibility under different experimental conditions. The results obtained from two analysis methods showed no significant deviation. The results obtained by the new established QAMS analytical method showed that the consistency of compound types among different batches of Psoraleae Fructus were better, but the content of different componounds was relatively different. Conclusion: The newly established QAMS analytical method for simultaneous determination of 16 compounds in Psoraleae Fructus provides a more efficient method to evaluate the comprehensive quality of Psoraleae Fructus from different sources.
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Objective: To establish quantitative analysis of multi-components by single marker (QAMS) method for simultaneous determining the content of seven saponins in Panacis Japonici Rhizoma, and to evaluate the adaptation and application of QAMS method in the quality control of Panacis Japonici Rhizoma. Methods: The relative factor (fs/i) of ginsenoside Rg1, Re, Rb1, pseudoginsenoside RT1, chikusetsusaponin IV and a were established by HPLC method with chikusetsusaponin V as internal standard, which were used to calculate the content of seven saponins in Panacis Japonici Rhizoma. Meanwhile, external standard method (ESM) was used to calculate the content of seven saponins. The difference between QAMS and ESM was analyzed to evaluate the accuracy of QAMS. Results: The fs/i of ginsenoside Rg1, Re, Rb1, pseudoginsenoside RT1, chikusetsusaponin IV and IVa were 1.286 7, 1.432 7, 0.966 6, 0.962 4, 1.207 2, and 0.938 4. There was no significant difference between the content of 10 batches of Panacis Japonici Rhizoma determined by QAMS and ESM. Conclusion: The established QAMS method is accurate and can be used for quantitative analysis and quality evaluation of the content of seven saponins in Panacis Japonici Rhizoma.
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Objective: On the basis of simultaneous determination of seven saponins in flower buds of Panax ginseng, a method of quantitative analysis of multi-components by single marker (QAMS) for the determination of seven saponins was established, and the feasibility of the method was verified. Methods: Using HPLC-UV, ten batches of dried P. ginseng flowers were used as the research object. Ginsenoside Re was used as internal reference to determine the relative correction factor of ginsenoside Rg1, Rg2, Rb1, Rc, Rb2 and Rd. The content of each component was measured by the traditional external standard method, and the difference between the calculated value and the measured value was compared to verify the feasibility and accuracy of the external standard method. Results: The relative correction factors of six ginsenoside Rg1, Rg2, Rb1, Rc1, Rb2, and Rd in P. ginseng flower were 1.07, 1.05, 0.81, 0.80, 0.64, and 0.84, respectively. The relative correction factors of six ginsenosides were reproducible in the 10 batches, the determiation of QAMS were not significantly different from those measured by the external standard method. Conclusion: In the case of shortage of ginsenoside reference substance, a method of QAMS can be used, the content of ginsenoside Rg1, Rg2, Rb1, Rb1, Rb2, and Rd in flower buds of P. ginseng can be determined by relative calibration factor.
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OBJECTIVE： To establish a method for simultaneous determination of α-pinene， β-pinene， limonene and α-terpineol in volatile oil of Forsythia suspensa. METHODS： GC method was adopted. The determination was performed on HP-5 capillary column through temperature-programmed route. The inlet temperature was 230 ℃， and detector temperature was 250 ℃； split sampling was applied （split ratio of 8 ∶ 1）； the air flow rate was 300 mL/min， the hydrogen flow rate was 30 mL/min， the tail gas flow rate was 30 mL/min， and the injection volume was 1 μL. Using limonene as internal reference， relative correction factors of α-pinene， β-pinene and α-terpineol were established， and the reproducibility of relative correction factors were investigated by using different chromatographs and columns， and chromatographic peak location of components was measured. The contents of above components were calculated with QAMS， and then compared with the results of external standard method. RESULTS： The linear range of α-pinene， β-pinene， limonene and α-terpineol were 16.5-990.0， 38.1-2 287.5， 8.2-491.2， 2.4-142.5 μg/mL， respectively （r≥0.999 1）. RSDs of precision， reproducibility and stability tests were all lower than 3％ （n＝6）. Average recoveries were 99.7％-105.5％（RSD＜4％，n＝9）. Compared with limonene （1.00），the average relative correction factors of α-pinene， β-pinene and α-terpineol were 0.91，0.86 and 1.11（n＝3）； relative retention time were 0.69-0.74， 0.81-0.86， 1.25-1.35（RSD＜3％，n＝3）. By using different chromatographs and columns， RSDs of relative correction factors were 0.21％-4.65％（n＝6）. Compared with external standard method， determination results of above 4 components were consistent （the absolute value of relative error were all less than 7％）. CONCLUSIONS： QAMS can be used for simultaneous determination of 4 kinds of effective components in volatile oil from F. suspensa.
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OBJECTIVE： To establish a method for simultaneous determination of 4 triglyceride anti-tumor components in Coix lacryma seed oil. METHODS： HPLC-ELSD was adopted. The determination was performed on Inertsil ODS-3 C18 column with mobile phase consisted of acetonitrile-isopropanol （57 ∶ 43， V/V） at the flow rate of 1.0 mL/min. The column temperature was 30 ℃， and the sample size was 10 μL. Evaporative light scattering detector was used， the drift tube temperature was 70 ℃， and the gas flow rate was 2 L/min. Using glycerol trioleateas internal standard， relative correction factors （RCF） of linolein trilinolein， 1，2-linoleic acid-3-palmitic acid glyceride and 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride were calculated respectively. The contents of above 3 components in C. lacryma seed oil were calculated by RCF. The contents of 4 components in C. lacryma seed oil were determined by external standard. The results of content determination by quatitative analysis of multi-components by single marker （QAMS） were compared with external standard method. RESULTS： The linear ranges were 0.15-4.50 μg for linolein trilinolein， 0.15-4.50 μg for 1，2-linoleic acid-3-palmitate， 0.35-10.50 μg for 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride， 0.35-10.50 μg for glycerol trioleate （r≥0.999 5）. The limits of quantification were 0.13， 0.06， 0.07， 0.12 μg. The limits of detection were 0.04， 0.02， 0.02， 0.03 μg， respectively. RSDs of precision， stability， and repeatability tests were less than 2.0％（n＝6）. The average recoveries were 95.43％-102.67％（RSD＜2.0％， n＝6）. Average RCFs of linolein trilinolein， 1，2- linoleic acid-3-palmitic acid glyceride and 1-palmitic acid-2- oleic acid-3-linoleic acid glyceride were 0.31， 0.88， and 1.21， respectively. RCFs reproducibility was perfect under different experiment conditions. There was no significant difference in results of content determination between QAMS and external standard method （P＞0.05）. CONCLUSIONS： The method is simple， rapid， accurate and reliable. It is used for simultaneous determination of linolein trilinolein， 1， 2-linoleic acid-3-palmitate， 1-palmitic acid-2-oleic acid-3-linoleic acid glyceride and glycerol trioleateas in C. lacryma seed oil.
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OBJECTIVE: To establish a method of quantitative analysis of multi-components by single marker (QAMS) for determining four essential oils (cinnamaldehyde, cinnamyl alcohol, cinnamic acid, 2-methoxy cinnamaldehyde) in Cinnamomum cassia, and provide the experimental base for establishing the quality standard of Cinnamomum cassia. METHODS: Cinnamaldehyde was used as the internal reference standard, and the relative correction factors (RCF) of cinnamyl alcohol, cinnamic acid, and 2-methoxy cinnamaldehyde in Cinnamomum cassia were calculated. The contents of the four components were determined by both external standard method and QAMS. The validity of the QAMS method was evaluated by comparison of the quantitative results of both methods. RESULTS: The RCFs had good reproducibility, relative correction factor 0.673, 0.605 and 1.943, with RSDs of 0.529%, 0.373%, and 0.759%, respectively. No significant differences were found in the quantitative analysis results of cinnamyl alcohol, cinnamic acid, 2-methoxy cinnamaldehyde by using RCF and ESM. CONCLUSION: In the absence of reference substance, the content determination of the four essential oils in Cinnamomum cassia can be realized by QAMS, and this method can be used in the multi-index evaluation of Cinnamomum cassia essential oil constituents. It is suggested that the standard for cinnamaldehyde content be increased to 2.5%, and the contents of total cinnamyl alcohol, cinnamic acid and 2-methoxy cinnamaldehyde be not less than 0.2%.
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OBJECTIVE： To establish a UHPLC method for determination of the contents of 11-keto-β-boswellic acid(KAB) and 11-keto-β-acetyl-boswellic acid(AKBA)in Frankincense and explore the suitability and accuracy of substitute reference substance method with DRS origin software for qualitative and quantitative determination of chromatographic peaks. METHODS ：The samples were separated by UHPLC for determination of AKBA and KBA. AKBA was used as a reference to investigate the accuracy of KBA identification using DRS origin software on 19 different C18 columns. The RSDs of relative correction factors were calculated for different detection wavelengths and instruments.The relative correction factor method and the external standard method were selected for quantification and the differences were compared. RESULTS: The established method met the requirements of methodology and the average recovery was 100.21%(n=6) with RSD of 2.47%. The DRS origin software can be used to accurately determine the chromatographic peaks. The correct factor of AKBA vs. KBA was 0.936 and it was consistent under different conditions. There were no significant differences between the content calculated by the relative correction factor method and by the external standard method. CONCLUSION： This method is intelligent, feasible, reliable and economical, and can be used for the determination of frankincense content.
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Objective:To establish a method of the quantitative analysis of multi-components by single-marker (QAMS)for the simultaneous determination of content of the 8 components, demethylwedelolactone, wedelolactone, juju-boside A, jujuboside B, betulinic acid, salidroside, ligustroflavone and specnuezhenide, in Anshen Yinao pills. Meth-ods: Anshen Yinao pills were used as the research object. With salidroside as an internal reference substance, the rela-tive correction factor for the other 7 components was established and the content of each component was calculated with each of the relative correction factors. Meanwhile, the content of each component was determined by the external standard (ES)method, and the content values from the ES and QAMS methods were compared to validate the accuracy and reli-ability of the QAMS method. Results: The eight components showed a good linearity within the given concentration rang-es(r≥0.9991). The average recovery for the eight components was in the range of 96.99-100.07%(n=9)with the RSD ranged in 0.67%-1.46%. The contents of the eight components showed no significant difference between the data mea-sured by the ES method and the data calculated by the QAMS method. Conclusion: The established method is simple and accurate, which could be used for quality evaluation of Anshen Yinao pills.
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In this study， quantitative analysis of multi-components with single marker(QAMS) was established and validated to simultaneously determine four sesquiterpenoids(β-eudesmol， atractylon， atractylolideⅠ， atractylolide Ⅱ) in Atractylodis Rhizome based on the gas chromatographic method(GC). Using β-eudesmol as the contrast， the relative correctionfactors(RCF) of the other three sesquiterpenoids were determined by GC. Within the line arranges，the values of RCF of β-eudesmol to atractylon， atractylolideⅠand atractylolide Ⅱ were 0.823， 0.690 and 0.766， respectively. The RCF had a good reproducibility in various instruments， chromatographic columns. According to their RCF， we simultaneously determined four sesquiterpenoids in Atractylodis Rhizome only using one marker. The results of QAMS method were validated by comparing with that of internal standard method， and no obvious significant difference was found.
Subject(s)
Atractylodes , Chemistry , Chromatography, Gas , Drugs, Chinese Herbal , Chemistry , Feasibility Studies , Phytochemicals , Reproducibility of Results , Rhizome , ChemistryABSTRACT
The present study is establish the quantitative analysis of multi-component with single marker for determining three anthroic acids, (25S)-antcin K, (25R)-antcin K and (25S)-antcin C in the petri dish cultured Antrodia camphorata. The relative correction factors of (25S)-antcin K and (25R)-antcin K were established by high performance liquid chromatography with (25S)-antcin C as the internal reference. Relative correction factors were used to calculate the contents of (25S)-antcin K and (25R)-antcin K which were difficult to gain in abundance. At the same time, the contents of these three compounds were determined by external standard method. Two methods were compared to evaluate the accuracy and rationality of the multi-components with single marker method in the determination of the petri dish cultured A. camphorate. It was found that the quantitative method of multi-component with single marker and external standard method showed no significant difference. In summary, taking (25S)-antcin C as the internal reference, the method of multi-component with single marker can be applied to the quantitative analysis of (25S)-antcin K and (25R)-antcin K in the petri dish cultured A. camphorata.
Subject(s)
Antrodia , Chemistry , Biomarkers , Cholestenes , Chromatography, High Pressure LiquidABSTRACT
Objective:To establish an analysis method for determining the contents of 7 components including ganoderic acid C2, ganoderic acid B,ganoderic acid G,ganoderic acid A,lucidenic acid A,ganoderma D and ganoderic acid F in ganoderma by QAMS. Methods:An HPLC method was used. The column was WatersX-bridge C18(250 mm × 4.6 mm, 5 μm), the mobile phase was acetonitrile(A)-1% acetic acid(B) (28:72) with gradient elution(0-30 min:A-28% to 38%;30-45 min:A-38% to 55%) at a flow rate of 1.0 ml·min-1,the column temperature was 30℃, and the detection wavelength was 254 nm. Ganoderic acid A was used as the internal reference, the correction factors of ganoderic acid C2, ganoderic acid B, ganoderic acid G, lucidenic acid A,ganoderma D and ganoderic acid F were calculated,and the contents of the 7 components were calculated by an external standard method to verify the feasibility and applicability of QAMS. Results:The relative correction factors of multiple assessments were reproducible,and the relative deviation of the contents of 6 components in 16 batches of Ganoderma lucidum was less than 2% when compared with that of the external standard method. Conclusion:QAMS is accurate and reliable in the quality evaluation of Ganoderma lucidum.