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Determination of 8 Glycosides and 4 Aglycones in Directionally Processed Astragalus membranaceus under Different Temperatures by UPLC-MS / 中国药房
China Pharmacy ; (12): 287-293, 2020.
Article in Chinese | WPRIM | ID: wpr-817331
ABSTRACT
OBJECTIVE:To establish a method for the determination of 8 glycosides(astragaloside Ⅰ,Ⅱ,Ⅲ,Ⅳ and calycosin glucopyranoside ,2′-hydroxy-3′,4′-dimethoxy-isoflavan-glucoside and 9,10-dimethoxy-pterocarpan-glucoside) and 4 aglycones(calycosin,formononetin,7,2′-dihydroxy-3′,4′-dimethoxy-isoflavan and 3-hydroxy-9,10-dimethoxy-pterocarpan) in Astragalus membranaceus ,and to investigate the effects of different processing temperatures on the contents of above 12 components. METHODS :The contents of 12 components in A. membranaceus and samples processed under different temperatures(120,140,160,180,200 ℃)were determined by UPLC-MS/MS. The determination was performed on ACQUITY UPLC HSS T 3 column with mobile phase consisted of 0.1 mol/L formic acid water solution -0.1 mol/L formic acid acetonitrile solution (gradient elution )at the flow rate of 0.5 mL/min. The column temperature was 30 ℃. The detection wavel ength was 260 nm,and sample size was 2 μL. Electrospray ion source(ESI)was used under positive ion mode (ESI+). The mass scanning range was mass ratio (m/z)of 50-1 500,with capillary voltage of 2 000 V and ion source temperature of 100 ℃. The desolvation temperature was 400 ℃;flow rate of atomizing gas (N2) was 40 L/h,and that of desolvation was 800 L/h;collision energy (CE)was 20-30 V;data acquisition rate was 0.5 s/scan. RESULTS:The linear range of astragaloside Ⅰ,astragaloside Ⅱ,astragaloside Ⅲ,astragaloside Ⅳ,calycosin-glucopyranoside, calycosin,ononin,formononetin,2′-hydroxy-3′,4′-dimethoxy-isoflavan-glucoside,7,2′-dihydroxy-3′,4′-dimethoxy-isoflavan,9, 10-dimethoxy-pterocarpan-glucoside and 3-hydroxy-9,10-dimethoxy-pterocarpan were 0.001 16-0.232 0,0.000 276-0.055 2, 0.000 22-0.044 0,0.000 225-0.045 0,0.000 734-0.587 0,0.001 17-0.234 0,0.000 742- 0.148 0,0.001 30-0.260,0.003 98-0.795 0, 0.000 476-0.476 0,0.001 89-0.378 0,0.000 336-0.336 0 μg(all R2≥0.999 2),respectively. The limits of detection were 6.2×10-6, 4.8×10-6,3.8×10-6,3.4×10-6,5.8×10-6,4.8×10-6,4.2×10-6,3.2×10-6,5.8×10-6,2.6×10-6,4.2×10-6,6.4×10-6 μg,respectively. The limits of quantitation were 12.6×10-6,16.2×10-6,14.4×10-6,14.8×10-6,18.8×10-6,16.4×10-6,15.4×10-6,10.8×10-6,20.2×10-6, 12.4×10-6,14.6×10-6,23.4×10-6 μg,respectively. RSDs of precision ,stability(24 h)and repetition tests were all lower than 3.0%(n=6). The average recoveries were 99.1%,100.2%,98.7%,101.9%,98.6%,102.1%,99.2%,100.3%,98.7%, 99.2%,99.3% and 100.8%,with the RSDs of 1.9%,2.2%,2.4%,1.8%,2.1%,1.7%,2.3%,1.9%,2.4%,1.8%,2.2% and 1.9%(n=6),respectively. The results showed that the contents of astragaloside Ⅰ,Ⅱ and Ⅲ decreased gradually with the increase of processing temperature ;the content of astragaloside Ⅳ increased gradually with the increase of temperature. The content of flavonoid glycosides ,such as calycosin glucopyranoside ,ononin,2′-hydroxy-3′,4′-dimethoxy-isoflavan-glucoside and 9, 10-dimethoxy-pterocarpan-glucoside decreased with the increase of temperature ;the corresponding aglycone components as flavonoid glycosides ,formononetin,3-hydroxy-9,10-dimethoxy- pterocarpan increased firstly and then decreased with the increase ; the content of 7,2′-dihydroxy-3′,4′- dimethoxy-isoflavan decreased with the increase of temperature. CONCLUSIONS :Established UPLC-MS/MS method can be used for determination of 12 components in A. membranaceus . After processed under different temperature,the contents of glycosides decreased in general ,while the contents of aglycones increased in general.

Full text: Available Index: WPRIM (Western Pacific) Language: Chinese Journal: China Pharmacy Year: 2020 Type: Article

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Full text: Available Index: WPRIM (Western Pacific) Language: Chinese Journal: China Pharmacy Year: 2020 Type: Article