18(100 mm×3.0 mm,1.8 μm)色譜柱;流動(dòng)相為乙腈(A)-0.1%甲酸水(B),梯度洗脫,體積流量0.2 mL/min;質(zhì)譜采用正、負(fù)離子掃描,掃描范圍m/z 100~2000。HPLC-MS/MS法采用Waters XBridge® BEH C18(150 mm×4.6 mm,2.5 μm)色譜柱;流動(dòng)相為乙腈(A)-0.1%甲酸水(B),梯度洗脫,體積流量0.4 mL/min;Scheduled MRM正負(fù)離子切換監(jiān)測(cè)模式定量分析。ig給予SD大鼠產(chǎn)復(fù)康顆粒(0.5、5 g/kg),給藥后于不同時(shí)間點(diǎn)頸靜脈取血0.2 mL,分離血漿,HPLC-MS/MS法檢測(cè)產(chǎn)復(fù)康顆粒入血成分及含量。結(jié)果 HPLC-TOF-MS法鑒定產(chǎn)復(fù)康顆粒中24種成分;建立的HPLC-MS/MS方法分離度良好,各方法學(xué)驗(yàn)證均符合要求,對(duì)13種主要成分進(jìn)行定量分析,水蘇堿、黃芪甲苷和益母草堿的含量較高,可能是其主要活性成分;藥動(dòng)學(xué)結(jié)果顯示,僅在給藥劑量5 g/kg時(shí),血漿中可檢測(cè)到水蘇堿和益母草堿,水蘇堿的消除較慢,益母草堿快速消除。結(jié)論 該方法簡(jiǎn)便、準(zhǔn)確,重復(fù)性好,可用于產(chǎn)復(fù)康顆粒中多種成分的鑒定和含量的測(cè)定,為藥材的質(zhì)量控制、藥動(dòng)學(xué)研究提供了參考。;Objective To establish qualitative and quantitative analysis methods for identification and determination of multi-constituent of Chanfukang granules (CFKG) using high performance liquid chromatography-time-of-flight mass spectrometry (HPLC-TOF-MS) and high performance liquid chromatography-triple quadrupole mass spectrometry (HPLC-MS/MS), and a preliminary pharmacokinetic study was carried out. Methods An Agilent ZORBAX Eclipse Plus C18 column (100 mm×3.0 mm, 1.8 μm) and a Waters XBridge® BEH C18 column (150 mm×4.6 mm, 2.5 μm) were used with 0.1% formic acid aqueous solution-acetonitrile as mobile phases by gradient elution. The compounds were detected by electrospray ion source in both positive and negative mode with multiple reaction monitoring (MRM) mode. SD rats were ig with CFKG (0.5, 5 g/kg). Blood samples of 0.2 mL were taken from jugular vein at different time points and plasma components and contents were determined by HPLC-MS/MS. Results Twenty-four constituents were identified by HPLC-TOF-MS qualitative analysis and thirteen constituents were quantitatively detected by HPLC-MS/MS. The established HPLC-MS/MS method had a good separation, and all the legal verification met the requirements. The content of stachydrine, Leonurine, and astragaloside IV were high, which may be the main active ingredient. The pharmacokinetic results showed that, only when the dose was 5 mg/kg, stachydrine and Leonurine can detected. Elimination of stachydrine was slow and elimination of Leonurine was fast. Conclusion A rapid and efficient method for studying the chemical constituents was established, which could provide reference for the quality control of Chanfukang granules."/>

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首頁 > 過刊瀏覽>2017年第40卷第11期 >2017,40(11):1559-1568. DOI:10.7501/j.issn.1674-6376.2017.11.007
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基于HPLC-TOF-MS和HPLC-MS/MS技術(shù)的產(chǎn)復(fù)康顆粒主要成分定性定量及藥動(dòng)學(xué)研究

Qualitative, quantitative and pharmacokinetic analysis of major constituents in Chanfukang granules by HPLC-TOF-MS and HPLC-MS/MS

發(fā)布日期:2017-11-15
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