1.Simultaneous determination of four constituents in Xiaojie'an Capsules by HPLC
Gang BAO ; Yamin ZUO ; Jianjun HUANG ; Tian ZHOU ; Wei PAN ; Qing WU ; Xing LI
Chinese Traditional Patent Medicine 2017;39(3):536-539
AIM To establish an HPLC method for the simultaneous content determination of four constituents in Xiaojie'an Capsules (Forsythiae Fructus,Leonuri Herba,Spatholobi Caulis,etc.).METHODS The analysis of chloroform extract of this drug was carried out on a 30 ℃ thermostatic Diamond C1scolumn(250 mm ×4.6 mm,5 μm),with the mobile phase comprising of acetonitrile (A)-0.05 mol/L monosodium phosphate (B) flowing at 1.0 mL/min in a gradient elution manner,and the detection wavelength was set at 278 nm.RESULTS Berberine hydrochloride,palmatine chloride,phillyrin and rutin showed good linear relationships within the ranges of 0.033 7-0.337 2 μg (r =0.999 1),0.054 8-0.548 3 μg (r =0.999 0),0.025 9-0.258 8 μg (r=0.999 2) and 0.008 4-0.084 2 μg (r =0.999 6),whose average recoveries were 98.8% (RSD =1.3%),99.8% (RSD =0.7%),98.8% (RSD =1.3%) and 96.8% (RSD =1.0%),respectively.CONCLUSION This sensitive and accurate method can be used for the quality control of Xiaojie'an Capsules.
2.Simultaneous Determination of 6 Ingredients in Polygonati Rhizoma and Its Decoction Piece by HPLC-QAMS
Yamin ZUO ; Chen LI ; Xingchun PENG ; Ronghua WEI ; Qing WU ; Yan ZHENG ; Xuehua DENG
China Pharmacy 2019;30(13):1748-1754
OBJECTIVE: To establish a quantitative analysis of multi-components by singer marker (QAMS) for determining the contents of diosgenin, 5-hydroxymethylfurfural, vanillic acid, rutin, quercetin, kaempferol in Polygonati Rhizoma and its decoction piece. METHODS: HPLC external standard method was used to determine the contents of 6 components in Polygonati Rhizoma and its decoction piece simultaneously [the separation was carried out on Diamonsil-C18 column with mobile phase consisted of acetonitrile-water (gradient elution); the detection wavelengths of 5-hydroxymethylfurfural, vanillic acid, rutin, quercetin and kaempferol were set at 254 nm(0-60 min); the detection wavelength of diosgenin was set at 202 nm (60-75 min) at the flow rate of 1.0 mL/min. The column temperature was 30 ℃]. Using vanillic acid as internal standard, relative correction factors (RCFs) of aother 5 components were calculated and to investigate durability. Relative retention method was used to accurately locate the chromatographic peaks of the components to be determined, and then the contents of the aother 5 components in Polygonati Rhizoma were calculated according to RCFs, and the results were compared with those determined by external standard method. The method was validated by Polygonati Rhizoma decoction piece. The contents of 6 components were determined by QAMS method and external standard method respectively, and then the differences of content determination were compared between 2 methods. RESULTS: The methodology investigation results of HPLC method were in line with related requirements. Within the linear range, the RCFs of diosgenin, 5-hydroxymethylfurfural, rutin, quercetin, kaempferol were 0.195, 0.025, 0.263, 0.345 and 0.075, respectively. Under different experiment conditions, RCFs showed good reproducibility; there was no statistical significance of 6 components in Polygonati Rhizoma and its decoction piece determined by external standard method and QAMS method (P>0.05). CONCLUSIONS: Established QAMS method is suitable for simultaneous determination of 6 components in Polygonati Rhizoma and its decoction piece.