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| Rapid determination of copper pyropheophytin-a in commercial olive oil by HPLC-MS/MS |
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| DOI：10.19902/j.cnki.zgyz.1003-7969.230193 |
| KeyWord:high performance liquid chromatography tandem mass spectrometry copper pyropheophytin-a olive oil adulteration |
| FundProject:天津市市场监督管理委员会科技计划项目（2022-W18）；天津市食品安全检测技术研究院新羽计划项目（SJY2022S01） |
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| Abstract: |
| An analytical method for determining copper pyropheophytin-a in olive oil utilizing high performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS) was established to accurately and quickly detect illegally added liposoluble pigments in commercial olive oil. Purification of the sample was performed using a SPE column for pre-treatment, followed by qualitative and quantitative detection using HPLC-MS/MS. The Chromatographic analysis was carried out on C8 column, with methanol-1 mol/L aqueous solution of ammonium acetate (volume ratio 8∶ 2) and methanol-acetone (volume ratio 6∶ 4) as mobile phases for gradient elution. Atmospheric pressure chemical ionization at negative ion mode and multi reaction monitoring scanning were used for mass spectrometry analysis under the conditions of electronic multiplication voltage 600 V and fragmentation voltage 260 V, and the analyte was quantified by external standard method. The results of the methodological validation showed that this method exhibited a limit of detection of 12 μg/kg and a limit of quantification of 64 μg/kg, with spiked recovery rates ranging from 91.0% to 106.0%, with relative standard deviations varying from 3.9% to 5.7%. This method had advantages of high sensitivity and precision, and can detect of copper pyropheophytin-a in olive oil rapidly. |
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