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Ultra-high performance liquid chromatography coupled with quadrupole/time-of-flight tandem mass spectrometry (UPLC-Q/TOF-MS/MS) has been used to detect the metabolites of schaftoside in plasma, bile, urine and feces of mice after oral administration. The study was approved by the Experimental Animal Ethics Committee from Xuzhou Medical University (No. XZMULL201612024). Compounds were identified by analyzing their high-resolution mass spectrometry data, mass spectra, and comparison with reference substances and the literatures. The parent compound and 29 metabolites were detected in the plasma, bile, urine and feces samples of mice. The main metabolic pathways of schaftoside in mice include deglycosylation/glycosylation, hydroxylation/dehydroxylation, hydrogenation, methylation, acetylation, sulfation, and glucuronidation. This study provides references for the material basis of schaftoside in vivo.
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Objective:To establish an HPLC method to determine the content of schaftoside in Jinshaniu Huashi tablets .Meth-ods:The separation was performed on an Agilent ZORBAX SB-C18 column(150 mm ×4.6 mm, 5 μm)with 0.2% phosphoric acid-acetonitrile as the mobile phase with gradient elution at a flow rate of 1.0 ml· min-1 .The detection wavelength was set at 272 nm, and the column temperature was set at 25 ℃.Results: The calibration curve of schaftoside had a good linearity within the range of 4.58-183.15 μg· ml-1(r=1.000 0).The average recovery was 99.65%with RSD of 1.09%(n=6).Conclusion:The established method is simple and accurate with high repeatability , which can be used for the content determination of schaftoside in Jinshaniu Hua-shi tablets .
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OBJECTIVE:To establish a method for simultaneous determination of vicexin 2,vicexin 1 and schaftoside in Shilin-tong tablet. METHODS:HPLC was performed on the column of Phenomenex C18 with mobile phase of methanol-0.1% phosphoric acid (gradient elution)at the flow rate of 0.8 ml/min,the detection wavelength was 334 nm,the column temperature was 25 ℃, and the injection volume was 10 μl. RESULTS:The linear range was 0.31-3.10 μg for vicexin 2 (r=0.9999),0.28-2.80 μg for vicexin 1(r=0.9999)and 0.39-3.90 μg for schaftoside(r=0.9999),respectively;RSDs of precision,stability and reproducibili-ty tests were lower than 3.0%;recoveries were 95.2%-100.4%(RSD=1.6%,n=9),96.3%-100.8%(RSD=1.4%,n=9) and 95.7%-100.9%(RSD=1.7%,n=9),respectively. CONCLUSIONS:The method is simple,sensitive ,accurate,reliable and repro-ducible,and can be used for the quality control of Shilintong tablet.
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Objective: This study is aimed to establish a high performance liquid chromatography coupled with quadrupole-time-of- flight mass spectrometric (HPLC-Q-TOF-MS) method for analyzing the main active components in Desmodii Styraciflii Herba, and to establish an HPLC-DAD method for simultaneously determining its seven flavonoids compounds (schaftoside, isoschaftoside, vicenin-2, isoorientin, isovitexin, luteolin, and apigenin). Methods: The analysis was performed on a Phenomenex Kinetex C18 column with a gradient elution of methanol-0.2% aqueous formic acid at the flow rate of 1.0 mL/min. The column temperature was 40 oC. The Q-TOF-MS discriminant analysis was performed under negative electrospray ion mode and the split ratio was 1∶1. Quantitative analysis of seven compounds in Desmodii Styraciflii Herba was carried by HPLC-DAD. The determination wavelength was at 272 nm. Results: Forty-one main active constituents were separated and identified by HPLC-Q-TOF-MS, including 37 flavonoids compounds and four phenolic acids. A HPLC-DAD method was successfully developed for determining seven flavonoids compounds. The standard curves for all seven compounds showed good linearity with correlation coefficients higher than 0.999 0 within the test ranges. The average recoveries (n = 6) were between 96.7%-102.4%, and RSD ≤ 4.94%. Conclusion: Analyzing the main active components provides a significant guidance for the substance basis research of Desmodii Styraciflii Herba. The HPLC-DAD method for simultaneously determining seven flavonoids compounds is accurate, reproducible, and provides the basis for the quality control of Desmodii Styraciflii Herba.
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ABSTARCT OBJECTIVE:To establish a method for the simultaneous determination of caffeic acid,isoschaftoside and schafto-side in Xiaoyan lidan tablet. METHODS:RP-HPLC was performed on the column of Phenomenex C18 with mobile phase of metha-nol- 0.1% phsphate acid(gradient elution)at flow rate of 0.8 ml/min,the detection wavelength was 334 nm,column temperature was 25 ℃,and the injection volume was 10 μl. RESULTS:The linear range was 0.10-2.81 μg for caffeic acid(r=0.999 9), 0.20-5.63 μg for isoschaftoside(r=0.999 9)and 0.10-2.63 μg for schaftoside(r=0.999 9);RSDs of precision,stability and repro-ducibility tests were lower than 3%;recoveries were 96.3%-100.4%(RSD=1.59%,n=9),97.3%-101.2%(RSD=1.28%,n=9) and 96.6%-100.6%(RSD=1.39%,n=9),respectively. CONCLUSIONS:The method is sensitive,accurate,reliable and reproduc-ible,and can be used for the simultaneous determination of caffeic acid,isoschaftoside and schaftoside in Xiaoyan lidan tablet the quality control of Xiaoyan lidan tablet.
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Objective:To establish an HPLC method for the simultaneous determination of viceninⅡ, isoschaftoside and schafto-side in Isodon lophanthoides, and analyze their content dynamic changes. Methods:The HPLC system consisted of a Phenomenex luna C18(250 mm ×4.6 mm, 5 μm)column and a solution system of methanol and 0.5% formic acid with gradient elution, the flow rate was 0. 8 ml·min-1 and the detection wavelength was 334 nm at the column temperature of 25℃and the injection volume was 10 μl. Results:The linear range of viceninⅡ, isoschaftoside and schaftoside was 0.130-3.110 μg(r =0.999 8), 0.180-4.540 μg(r =0.999 9) and 0.080-1.970 μg(r =0. 9999), respectively. The average recovery was 96.8% (RSD =1.9%), 99.2% (RSD =1. 6%) and 97. 1% (RSD=1. 6%) (n=6), respectively. The above three kinds of water-soluble flavonoids from seedling stage to significant accumulation, isoschaftoside and schaftoside reached the highest value in March and August, the content of VitexinⅡ in January and April tends to be stable, in May began to increase gradually, reached the maximum value in August, then began to de-crease. Conclusion:With the contents of water-soluble flavonoids as the indicators, the best harvest time of Isodon lophanthoides is March and August, and the quality of the medicinal materials harvested in August is the best.
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Objective:To establish an HPLC method for determining four constituents ( schaftoside, isoschaftoside, deoxyelephan-topin and 4,5-dicaffeoylquinic acid) in Shennongcha granules. Methods:An HPLC method was performed on a Hypersil C18 column (200 mm × 4. 6 mm,5 μm) with the mobile phase of acetonitrile as the phase A and 0. 025 mol·L-1 phosphoric acid solution as the phase B with gradient elution. The flow rate was 1. 3 ml·min-1 . The detection wavelength was set at 270 nm for schaftoside and isos-chaftoside, 208 nm for deoxyelephantopin and 327 nm for 4, 5-dicaffeoylquinic acid. The column temperature was room temperature. Results:The calibration curve was linear over the concentration range of 5. 850-117. 000 μg·ml-1 for schaftoside, 4. 650-93. 000 μg ·ml-1 for isoschaftoside, 4. 160-83. 200 μg · ml-1 for deoxyelephantopin and 5. 470-109. 400 μg · ml-1 for 4, 5-dicaffeoylquinic acid. The correlation coefficient of all curves was more than 0.999. The average recoverywas 97.70% (RSD=1.40%), 96.87%(RSD=1.13%), 97.53%(RSD =1.69%) and 99.29%(RSD =1.01%) (n =6) , respectively. Conclusion: The developed HPLC method is simple,accurate,and can be used in the content determination of Shennongcha granules.
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Objective: To investigate the water-soluble constituents of Isodon lophanthoides var. gerardianus. Methods: Compouds were isolated and purified by D-101, Sephadex LH-20, and ODS column chromatographies. The chemical structures were elucidated on the basis of spectral data and physicochemical properties. Results: Twelve compounds were isolated and identified as vitexin II (1), vicenin III (2), isoschaftoside (3), schaftoside (4), vitexin (5), 6, 8-di-C-α-L-arabinosylapigenin (6), apigenin-7-O-glucuronide (7), apigenin 6-C-β-L-arabin-osyl-8-C-α-L-arabinopyranoside (8), apigenin 6-C-β-D-xylopyranosyl-8-C-α-L-arabinopyranoside (9), caffeic acid (10), rosmarinic (11), and rutin (12). Conclusion: Compounds 1-9 are separated from I. lophanthoides var. gerardianus for the first time, and constituents of the water-soluble parts of I. lophanthoides var. gerardianus are studied systematically for the first time. Compounds 1, 6, and 11 exert antiproliferative effects on HepG2 cells.
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Objective To study the influence of climate, geographical environment and harvesting time on contents of schaftoside in Desmodium styracifolium Herba. Methods Content of schaftoside in Desmodium styracifolium Herba was determined by using HPLC. ODS-C18 column (4. 6 mmí250 mm,5 μm) was used, the mobile phase was methanol-water (3268), the detection wavelength was 272 nm, the flow rate was 0. 5 mL·min-1, and the column temperature was 35℃. Results The climate type, amount of precipitation, average temperature, duration of sunshine, geographical environment of different province had significant impacts on the content of schaftoside in Desmodium styracifolium Herba. Conclusion Subtropical monsoon climate, temperature from 25 ℃ to 32 ℃, sunshine time of 10 h per day and the average annual rainfall of 1 942 mm are suitable for growth of Desmodium styracifolium. The content of schaftoside in samples cultivated from Guangxi Province is higher than that cultivated from Guangdong Province and Hainan Province. The schaftoside content of sample cultivated in July is higher than that cultivated in other months.
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OBJECTIVE:To establish the identification method of Rhizoma Arisaematis and content determination of flavon-oids.METHODS:TLC was used to identify Rhizoma Arisaematis with schaftoside and ischaftoside as reference substances.The content of flavonoids was determined by HPLC.RESULTS:TLC of test sample and that of control substance had same color dots.The linear range of schaftoside and isoschaftoside were 7.925～126.8 ?g?mL-1(r=0.999 9) and 3.996～63.94 ?g?mL-1(r=0.999 7) respectively.Average recoveries were 99.4% for schaftoside (RSD=2.10%,n=9) and 99.52% for isoschaftoside(RSD=2.42%,n=9).CONCLUSION:The method is simple,accurate and reproducible for the quality evaluation of Rhizoma Arisaematis.