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An HPLC-MS/MS method was established for the simultaneous determination of 15 components [betaine, agaritol, bergamolide, 2-(2-phenylidene) chromone, dehydrodiisoeugenol, D-(-)-quinic acid, gallic acid, protocatechuic acid, hydroxysafflor yellow A, rutin, isoquercetin, ellagic acid, luteolin and apigenin] in Qingxin Chenxiang Bawei powder (pills). The quantitative method, combined with chemometrics and entropy weight-grey correlation degree method to analyze the comprehensive quality, provides a reference for the quality control and evaluation of this preparation.
The analysis was conducted using a Shim-pack GIST-HP C18 chromatographic column, with the mobile phase consisting of methanol (A) and a 0,1% formic acid aqueous solution (B). A gradient elution was employed at a column temperature of 35 ℃, with an injection column of 3 μL. Weisenxin platform was used for cluster analysis (CA), SIMCA 14.1 software was used for principal component analysis (PCA) and orthogonal partial least squares discriminant analysis (OPLS-DA), and the compounds with variable important in projection (VIP) value greater than 1.0 were used as the criterion to screen quality differences. The entropy weight-correlation degree method was used to analyze the comprehensive quality.
The linear relationship of the 15 components was good in their respective ranges, and the linear correlation r was greater than or equal 0.999 0. Precision RSD were all lower than 3.00%. The stability and repeatability were good, RSD lower than 5.00%; The average recoveries were 93.62%~105.10%, and RSD was 1.18%~4.37%. CA and PCA analysis classified 14 batches of Qingxin Chenxiang Bawei powder (pills) into 2 categories: manufacturers D (D1~D4) were grouped into one group, manufacturers A and M (A1~A4, M1~M6) were grouped into one group. Six difference markers were screened in OPLS-DA mode, which were D-(-)-quinic acid, agaritol, 2-(2-phenylethyl) chromone, dehydrodiisoeugenol, bergamolactone and quercetin, respectively. A2 has the best comprehensive quality.
The established HPLC-MS/MS method for the simultaneous determination of 15 components in Qingxin Chenxiang Bawei powder (pill) can be used for the comprehensive quality study of Qingxin Chenxiang Bawei powder (pill) combined with chemometrics and entropy weight correlation degree method.
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| 科 Family | 属数 Number of genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) | 属 Genus | 种数 Number of species | 占总种数比例 Percentage of total species (%) |
|---|---|---|---|---|---|---|
| 鹅膏菌科Amanitaceae | 2 | 11 | 5.26 | 鹅膏菌属 Amanita | 10 | 4.78 |
| 小菇科 Mycenaceae | 2 | 12 | 5.74 | 丝盖伞属 Inocybe | 5 | 2.39 |
| 多孔菌科 Polyporaceae | 8 | 14 | 6.70 | 蜡蘑属 Laccaria | 5 | 2.39 |
| 红菇科 Russulaceae | 3 | 23 | 11.00 | 小皮伞属 Marasmius | 6 | 2.87 |
| 小菇属 Mycena | 11 | 5.26 | ||||
| 光柄菇属 Pluteus | 5 | 2.39 | ||||
| 红菇属 Russula | 17 | 8.13 | ||||
| 栓菌属 Trametes | 5 | 2.39 |
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