ABSTRACT
OBJECTIVE To establish the method for simultaneous determination of 11 components as narirutin in Biantong capsules，to conduct chemical pattern recognition analysis and to screen differential markers affecting their quality . METHODS HPLC method was adopted . The separation was carried out on Venusil XBP C 18 column with mobile phase consisted of acetonitrile - 0.1％ phosphoric acid solution with gradient elution at flow rate of 1.0 mL/min. The sample size was 10 µL，and column temperature was set at 30 ℃. The detection wavelengths were set at 283，330，520，220 nm，respectively. Using verbascoside as an internal standard ，the contents were determined by quantitative analysis of mult -components by single marker （QAMS），and the results were compared with those of external standard method . Cluster analysis ，principle component analysis and orthogonal partial least squares -discriminant analysis were performed with SPSS 26.0 and SIMCA 14.1 software. The differential markers affecting the quality of Biantong capsules were screened using the variable importance in projection （VIP）value greater than 1 as the standard . RESULTS The contents of narirutin ，naringin，neohesperidin，echinacoside，tubuloside A ，isoacteoside，cyanidin-3-O-glucoside， cyanidin-3-O-rutoside，atractylolide Ⅲand atractylolide Ⅰ were 0.739-1.265，1.134-2.158，1.407-2.359，1.368-2.502，0.304-0.522， 0.257-0.521，0.423-0.727，0.375-0.733，0.130-0.283 and 0.062-0.166 mg/g，respectively. The relative average deviation of them from the external standard method was less than 2％. The results of cluster analysis showed that 15 batches of samples could be grouped into three categories ，S1-S7 as a category ，S8-S10 as a category ，and S 11-S15 as a category ，which was consistent with the classification results of principal component analysis . The results of orthogonal partial least squares -discriminant analysis showed that the VIP values of cyanidin -3-O-rutoside，atractylolide Ⅲ， naringin，neohesperidin，echinacoside and verbascoside were all greater than 1. CONCLUSIONS The method for simultaneous determination of 11 components in Biantongcapsules， including narirutin ， is successfully established . Combined with chemical pattern recognition analysis ，it can be used for the quality control of Biantong capsules . Six components such as cyanidin -3-O-rutoside may be the differential markers that affect the quality of Biantong capsules .
ABSTRACT
Objective:To identify the quality differential markers of different processed products of Glycyrrhiza uralensis dry roots and rhizomes. Method:Ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MSE) was used to collect high-precision mass-charge ratio and ion response strength information of the components in G. uralensis dry roots and rhizomes before and after processing by negative ion mode. The data set collected after pretreatment was analyzed with principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) to quickly search the differential components in different processed products of G. uralensis dry roots and rhizomes. Differential components were identified according to the relative molecular weight, fragment ion, mass spectrum database and related literature information, then the migration of components before and after processing was studied. Result:A total of 10 quality differential markers were searched from raw products, roasted products and honey-roasted products of G. uralensis dry roots and rhizomes, mainly derivatives of liquiritin and glycyrrhizic acid. Among them, the contents of 6''-O-acetylliquiritin apioside, 6''-O-acetylliquiritin apioside isomer, 6''-O-acetylliquiritin, formononetin and 11-deoxo-18β-glycyrrhetic acid were the highest in the raw products, the contents of 6''-O-acetylisoliquiritin apioside, 6''-O-acetylisoliquiritin, isoliquiritin and glycyrrhetic acid 3-O-glucuronide were the highest in the roasted products, the content of liquiritin was the lowest in the honey-roasted products. Conclusion:There are some chemical differences among the three products. This study can provide material basis for the quality control and pharmacodynamic research of processed products of G. uralensis dry roots and rhizomes.