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  • Author or Editor: Jun Zhao x
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Abstract

A rapid and simple method for the determination of stearic acid and 12-hydroxystearic acid in PEG-60 hydrogenated castor oil by high performance liquid chromatography with evaporative light scattering detection was established. The oil sample was first pretreated by alkaline hydrolysis. The analysis was performed on a Zhongpu Develop XD-C18 column (250 mm × 4.6 mm, 5 µm) with gradient elution of methanol and 1% acetic acid aqueous solution at a flow rate of 1.2 mL·min−1 and a column temperature of 40 °C. The drift tube temperature of the evaporative light scattering detection system was set at 40 °C, and the pressure of carrier gas (N2) was 337 kPa. The regression equation revealed a good linear relation (r = 0.9993–0.9995) during the test ranges (119.1–1190.7 μg·mL−1 for 12-hydroxystearic acid, 10.7–107.4 μg·mL−1 for stearic acid). The detection limits of 12-hydroxystearic acid and stearic acid were 1.1 and 2.5 μg·mL−1, the limits of quantitation were 3.2 and 7.4 μg·mL−1, respectively. And the mean recoveries were 101.5 and 101.0%, the corresponding relative standard deviations (RSDs) were 2.1 and 2.8%, respectively. The RSDs corresponding to repeatability (n = 6) were both less than 1.7% in terms of precision. As to the stability, the test results remained stable after 8 h at room temperature (RSDs were both less than 2.6%). The developed method showed high sensitivity, recovery, repeatability and stability, which indicated that the method could be applied as a quality evaluation method for the determination of stearic acid and 12-hydroxyoctadecanoic acid in PEG-60 hydrogenated castor oil.

Open access

Abstract

Atractylodis macrocephalae rhizome (AMR) belongs to medicine food homology. Its' clinical application of invigorating the spleen-stomach of AMR was applied to various diseases. In this research, a UPLC-QTOF-MS method was developed for qualitative and quantitative analysis of AMR, simultaneously. A Waters Acquity BEH C18 column (2.1 mm × 100 mm, 1.7 μm particle size) was used for separation of AMR multi-components. The column was eluted with a mobile phase of 0.1% formic acid-water and 0.1% formic acid-acetonitrile. Electron spray ionization with positive-ion mode and external standard method was utilized for quantifying the nine analytes in AMR. Constituents of AMR were scanned by UPLC-QTOF-MS and then identified by mass fragments and chromatographic information compared with the published literature and reference standards. Under positive mode, a total of 61 chemical compositions including 16 terpenoids, 8 polyacetylenes, 6 aromatics, 5 flavonoids, 5 coumarins, 5 organic acids, 4 amino acids, 3 fatty acids, 3 aliphatics, 2 steroids, and 2 alkenes, a nucleoside and an aldehyde were identified. Simultaneously, the contents of three amino acids (L-tyrosine, L-phenylalanine, and L-tryptophan), three sesquiterpenoids (atractylenolide Ⅲ, atractylenolide Ⅱ, and atractylenolide Ⅰ), a flavonoid (rutin), an organic acid (ferulic acid), and a pentacyclic triterpenoid (oleanolic acid) were determined in seventeen AMR batches. Amino acids and triterpenoid were quantified for the first time in AMR. The UPLC-QTOF-MS method developed in this article was reliable, practical, and useful for qualitative and quantitative evaluation of AMR multi-components.

Open access