کد مقاله کد نشریه سال انتشار مقاله انگلیسی نسخه تمام متن
1220749 1494624 2015 7 صفحه PDF دانلود رایگان
عنوان انگلیسی مقاله ISI
Unexpected retention behavior of baicalin: Hydrophilic interaction like properties of a reversed-phase column
موضوعات مرتبط
مهندسی و علوم پایه شیمی شیمی آنالیزی یا شیمی تجزیه
پیش نمایش صفحه اول مقاله
Unexpected retention behavior of baicalin: Hydrophilic interaction like properties of a reversed-phase column
چکیده انگلیسی


• Problem of an interfering peak occurred and solved during method development.
• Inverse gradient on a reversed phase column was used.
• LC–MS/MS method was developed to quantify baicalin in membrane vesicles.

The original aim of this study was to develop a method for the determination of baicalin from membrane vesicles. The unconventional chromatographic separation (“inverse gradient elution” on a reversed phase column) was due to a lucky chance, which is detailed and discussed in this study. The validated liquid chromatography-tandem mass spectrometry (LC–MS/MS) method is proved to be sensitive, rapid and selective. Chromatographic separation was performed on a Zorbax SB-C8 column (250 mm × 4.6 mm, i.d.; 5 μm) with 0.1% formic acid in water and methanol by linear gradient elution. Quantification of baicalin was determined by multiple reaction monitoring (MRM) mode using electrospray ionization (ESI). The calibration curve was linear (r = 0.9987) over the concentration range from 1 to 1000 nM. The coefficient of variation and relative error of baicalin for intra- and inter-assay at three quality control (QC) levels were 2.0–10.2% and −6.1 to 6.7%, respectively. The lower limit of quantification (LLOQ) for baicalin was 1 nM (0.446 ng/ml), without preconcentration of the sample. This method was subsequently applied to vesicular transport assays of baicalin in membrane vesicles successfully. The developed method can open up new area of research in the chromatographic separation of flavonoids and their glucuronides.

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ناشر
Database: Elsevier - ScienceDirect (ساینس دایرکت)
Journal: Journal of Pharmaceutical and Biomedical Analysis - Volume 111, 10 July 2015, Pages 119–125
نویسندگان
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