18(2)色譜柱(250 mm×4.6 mm,5 μm);流動相:0.2%甲酸水溶液–乙腈,梯度洗脫,檢測波長265、327 nm,體積流量1.0 mL/min,柱溫25℃,進樣量10 μL。液路采用三通分流0.2 mL/min進入ESI源,在正、負離子模式下進行質譜檢測。采用甲酸鈉溶液作為內參校準液每針校正。根據對照品、文獻報道和數(shù)據庫數(shù)據推測鑒定相關色譜峰的化合物和單味藥來源。結果 提取出85個基峰離子,根據元素分析推測出其化學式,其中80個推測出了可能的化合物結構信息,采用對照品確證了6個成分,其中歸屬于甘草、黃芩、大棗、黃連、干姜、半夏分別為40、31、13、11、5、1個成分。結論 HPLC-QTOF/MS作為一種高選擇性、高分離度、高靈敏度的分析手段能有效地鑒定甘草瀉心湯中化學成分。;Objective To identify the chemical constituents in Gancao Xiexin Decoction. Methods GancaoXiexin Decoction, single herb decoction and mixed reference substance were analyzed on HPLC C18 column (250 mm×4.6 mm, 5 μm) with the mobile phase 0.2% formic acid- acetonitrile at a flow rate of 1.0 mL/min. Detection wavelengths were set at 265 and 327 nm, volume flow rate was 1.0 mL/min, column temperature was 25 ℃, and sample injection volume was 10 μL. The fluid was infused into the ESI source at a flow rate of 0.2 mL/min by a tees,and was scanned in positive and negative ion mode by MS2. Sodium formate solution was used as internal standard. The compound attribution of related chromatographic peaks and the source of single herb were deduced and identified by comparison with the standard, literature, and database. Results Base peak chromatogram ions (85) were extracted and chemical formulas were deduced by elemental analysis, of which 80 constituents were deduced, and 6 constituents were confirmed using reference substances. Glycyrrhizae Radix et Rhizoma, Scutellariae Radix, Jujubae Fructus, Coptidis Rhizoma, Zingiberis Rhizome, and Pinelliae Rhizoma contributed 40, 31, 13, 11, 5, and 1 constituents, respectively. Conclusion HPLC-QTOF/MS can be applied in identification of constituents in Gancao Xiexin Decoction as a high selectivity, high resolution, and high sensitivity method."/>

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首頁 > 過刊瀏覽>2021年第36卷第11期 >2021,36(11):2246-2254. DOI:10.7501/j.issn.1674-5515.2021.11.005
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HPLC-QTOF/MS法鑒定甘草瀉心湯中化學成分

Identification of chemical constituents in Gancao Xiexin Decoction by HPLC-QTOF/MS

發(fā)布日期:2021-11-23