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Analysis of nine compounds from Alpinia oxyphylla fruit at different harvest time using UFLC-MS/MS and an extraction method optimized by orthogonal design.

Li YH, Chen F, Wang JF, Wang Y, Zhang JQ, Guo T - Chem Cent J (2013)

Bottom Line: The highest yield of nine compounds was achieved with 70% ethanol-water and a solvent-to-sample ratio of 20:1 at 60°C for 30 min.The contents of the six bioactive compounds were reported in A. oxyphylla for the first time.The contents of nine compounds of different harvest time fruits of A. oxyphylla were assessed under the optimized extraction and UFLC-MS/MS analytical conditions, and the 45-day culture fruit had the highest content levels.

View Article: PubMed Central - HTML - PubMed

Affiliation: Hainan Provincial Key Laboratory of R&D on Tropical Herbs, Hainan Medical University, Haikou 571199, China ; School of Pharmacy, Hainan Medical University, Haikou, Hainan 571199, China.

ABSTRACT

Background: The dried fruits of Alpinia oxyphylla Miq have been widely used as an herbal medicine for the treatment of diarrhea and enuresis in China. Medicinal chemistry studies revealed that the tepenes, diphenylheptanes and flavones were the main components. Therefore, these three kinds of components should be chosen as the bioactive marker compounds for the quality control of A. oxyphylla fruits. Moreover, multiple active components has been widely recognized to be a more feasible method for the quality control of herbal medicines. This study firstly provided a better method for comprehensive component analysis of A. oxyphylla fruits. Meanwhile, the different harvest time was also evaluated.

Results: The solvent-to-sample ratio was the most important factor comparing with solvent, extraction time and temperature. The highest yield of nine compounds was achieved with 70% ethanol-water and a solvent-to-sample ratio of 20:1 at 60°C for 30 min. The optimized analytical method for ultra fast high performance liquid chromatography (UFLC) was a gradient elution using water containing 0.04‰ formic acid (A) and methanol containing 0.04‰ formic acid (B), at a flow rate of 0.3 mL/min. Using this optimized method, nine compounds were simultaneously separated and quantified by UFLC coupled with tandem electro-spray ionized mass spectrometry (MS/MS).

Conclusions: The contents of the six bioactive compounds were reported in A. oxyphylla for the first time. The contents of nine compounds of different harvest time fruits of A. oxyphylla were assessed under the optimized extraction and UFLC-MS/MS analytical conditions, and the 45-day culture fruit had the highest content levels.

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Related in: MedlinePlus

Typical LC-MS/MS chromatograms of nine phytochemicals from A. oxyphylla fruit sample. They were identified by the comparison of the retention time and mass spectra (MRM mode) with the corresponding pure compounds.
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Figure 2: Typical LC-MS/MS chromatograms of nine phytochemicals from A. oxyphylla fruit sample. They were identified by the comparison of the retention time and mass spectra (MRM mode) with the corresponding pure compounds.

Mentions: MS spectra were studied in both positive and negative ion modes. It was found that compared to the negative ion mode, yakuchinone A and yakuchinone B had higher sensitivity in the positive ion mode, which made it easier to detect their contents in A. oxyphylla fruits, and easier to confirm molecular ions or protonated molecule ions in the identification of each peak. As such, the positive MS ion mode was selected. The chemical structures of nine components were characterized based on their retention behaviors and MS information, such as quasi-molecular ions [M + H]+ and fragment ions. The ion pairs of precursor-to-product for MRM detection were generated by the Compound Optimization which was embedded in the Analyst software. Each compound was investigated individually to achieve optimal scan time, DP, EP, CE and CXP. Under the optimized UFLC and MS/MS conditions, all nine compounds in the fruits of A. oxyphylla were identified and quantified. Retention time and MS information for each analyte including [M + H]+, quantitative ions, scan time, DP, EP, CE and CXP are shown in Table 1, and UFLC–MS/MS chromatograms of 9 markers in Figure 2.


Analysis of nine compounds from Alpinia oxyphylla fruit at different harvest time using UFLC-MS/MS and an extraction method optimized by orthogonal design.

Li YH, Chen F, Wang JF, Wang Y, Zhang JQ, Guo T - Chem Cent J (2013)

Typical LC-MS/MS chromatograms of nine phytochemicals from A. oxyphylla fruit sample. They were identified by the comparison of the retention time and mass spectra (MRM mode) with the corresponding pure compounds.
© Copyright Policy - open-access
Related In: Results  -  Collection

License
Show All Figures
getmorefigures.php?uid=PMC3750461&req=5

Figure 2: Typical LC-MS/MS chromatograms of nine phytochemicals from A. oxyphylla fruit sample. They were identified by the comparison of the retention time and mass spectra (MRM mode) with the corresponding pure compounds.
Mentions: MS spectra were studied in both positive and negative ion modes. It was found that compared to the negative ion mode, yakuchinone A and yakuchinone B had higher sensitivity in the positive ion mode, which made it easier to detect their contents in A. oxyphylla fruits, and easier to confirm molecular ions or protonated molecule ions in the identification of each peak. As such, the positive MS ion mode was selected. The chemical structures of nine components were characterized based on their retention behaviors and MS information, such as quasi-molecular ions [M + H]+ and fragment ions. The ion pairs of precursor-to-product for MRM detection were generated by the Compound Optimization which was embedded in the Analyst software. Each compound was investigated individually to achieve optimal scan time, DP, EP, CE and CXP. Under the optimized UFLC and MS/MS conditions, all nine compounds in the fruits of A. oxyphylla were identified and quantified. Retention time and MS information for each analyte including [M + H]+, quantitative ions, scan time, DP, EP, CE and CXP are shown in Table 1, and UFLC–MS/MS chromatograms of 9 markers in Figure 2.

Bottom Line: The highest yield of nine compounds was achieved with 70% ethanol-water and a solvent-to-sample ratio of 20:1 at 60°C for 30 min.The contents of the six bioactive compounds were reported in A. oxyphylla for the first time.The contents of nine compounds of different harvest time fruits of A. oxyphylla were assessed under the optimized extraction and UFLC-MS/MS analytical conditions, and the 45-day culture fruit had the highest content levels.

View Article: PubMed Central - HTML - PubMed

Affiliation: Hainan Provincial Key Laboratory of R&D on Tropical Herbs, Hainan Medical University, Haikou 571199, China ; School of Pharmacy, Hainan Medical University, Haikou, Hainan 571199, China.

ABSTRACT

Background: The dried fruits of Alpinia oxyphylla Miq have been widely used as an herbal medicine for the treatment of diarrhea and enuresis in China. Medicinal chemistry studies revealed that the tepenes, diphenylheptanes and flavones were the main components. Therefore, these three kinds of components should be chosen as the bioactive marker compounds for the quality control of A. oxyphylla fruits. Moreover, multiple active components has been widely recognized to be a more feasible method for the quality control of herbal medicines. This study firstly provided a better method for comprehensive component analysis of A. oxyphylla fruits. Meanwhile, the different harvest time was also evaluated.

Results: The solvent-to-sample ratio was the most important factor comparing with solvent, extraction time and temperature. The highest yield of nine compounds was achieved with 70% ethanol-water and a solvent-to-sample ratio of 20:1 at 60°C for 30 min. The optimized analytical method for ultra fast high performance liquid chromatography (UFLC) was a gradient elution using water containing 0.04‰ formic acid (A) and methanol containing 0.04‰ formic acid (B), at a flow rate of 0.3 mL/min. Using this optimized method, nine compounds were simultaneously separated and quantified by UFLC coupled with tandem electro-spray ionized mass spectrometry (MS/MS).

Conclusions: The contents of the six bioactive compounds were reported in A. oxyphylla for the first time. The contents of nine compounds of different harvest time fruits of A. oxyphylla were assessed under the optimized extraction and UFLC-MS/MS analytical conditions, and the 45-day culture fruit had the highest content levels.

No MeSH data available.


Related in: MedlinePlus