以QuEChERS方法搭配液相層析質譜技術定量紅酒樣品中的白藜蘆醇
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2017
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白藜蘆醇被證實有抗癌、抗發炎、抗心血管疾病等功效，甚或能調節新陳代謝、延長壽命。為定量白藜蘆醇，本實驗測試兩種樣品前處理方式：稀釋法以及一個快速、簡單、便宜、高效、穩固、便宜（QuEChERS）的萃取法。為能達到最佳萃取效率，我們針對紅酒樣品，優化QuEChERS萃取法之參數。最後選用1:1作為紅酒稀釋之比例、100%的乙腈作為液相萃取之溶劑，並混合300 mg一級二級胺（PSA）與300 mg無水硫酸鎂（MgSO4）作為分散式固相萃取（dSPE）之粉劑。接著，我們將稀釋法和優化後的QuEChERS萃取法，搭配高效能液相層析及串聯式質譜儀（HPLC-MS/MS），並對此二方法進行確效。QuEChERS搭配LC-MS/MS方法之線性範圍為5-500 ppb，最低偵測極限（LOD）為2.5 ppb、最低定量極限（LOQ）為5 ppb；其線性範圍與感度皆優於稀釋法。實驗中，使用兩不同前處理方式的回收率介於97.4%至111.3%，且相對標準差（RSD）皆小於4.9%（n=3）。最終，本實驗利用此二法檢測7種自市面上購得的紅酒樣品。在經檢出的3個樣品中，白藜蘆醇濃度介於5.5到498 ppb。本論文首度使用QuEChERS萃取法搭配LC-MS/MS技術進行紅酒中白藜蘆醇的定量分析研究。
Resveratrol (3,5,4'-trihydroxy-trans-stilbene) has been proved to be anti-cancer, anti-inflammatory, cardiovascular protective and is probably able to promote metabolism as well as prolonging life of human beings. In this study, two preparation strategies, including direct dilution and a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction, were examined for the quantification of resveratrol in red wines. A 1:1 wine/water dilution, 100% acetonitrile as LLE solvent, 300 mg primary and secondary amines (PSA) plus 300 mg anhydrous magnesium sulfate (MgSO4) as dSPE sorbent were found to give the best results. The dilution and optimal QuEChERS method combined with high performance liquid chromatography – mass spectrometry (HPLC-MS/MS) were further validated. A linear range between 5-500 ppb with LOD at 2.5 ppb and LOQ at 5.0 ppb by QuEChERS method are achieved, that shows broader linear range and superior sensitivity in comparison with dilution approach. The recoveries with the two preparation strategies ranged from 97.4% to 111.3% with RSD ≤ 4.9% (n=3). Eventually, resveratrol were detected in 3 out of 7 red wines from local markets, with concentrations within 5.5 to 498 ppb. To the best of our knowledge, this is the first report that combines efficient QuEChERS extraction with LC-MS/MS for the quantification of resveratrol in red wines.
Resveratrol (3,5,4'-trihydroxy-trans-stilbene) has been proved to be anti-cancer, anti-inflammatory, cardiovascular protective and is probably able to promote metabolism as well as prolonging life of human beings. In this study, two preparation strategies, including direct dilution and a quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction, were examined for the quantification of resveratrol in red wines. A 1:1 wine/water dilution, 100% acetonitrile as LLE solvent, 300 mg primary and secondary amines (PSA) plus 300 mg anhydrous magnesium sulfate (MgSO4) as dSPE sorbent were found to give the best results. The dilution and optimal QuEChERS method combined with high performance liquid chromatography – mass spectrometry (HPLC-MS/MS) were further validated. A linear range between 5-500 ppb with LOD at 2.5 ppb and LOQ at 5.0 ppb by QuEChERS method are achieved, that shows broader linear range and superior sensitivity in comparison with dilution approach. The recoveries with the two preparation strategies ranged from 97.4% to 111.3% with RSD ≤ 4.9% (n=3). Eventually, resveratrol were detected in 3 out of 7 red wines from local markets, with concentrations within 5.5 to 498 ppb. To the best of our knowledge, this is the first report that combines efficient QuEChERS extraction with LC-MS/MS for the quantification of resveratrol in red wines.
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白藜蘆醇, QuEChERS, 液相層析-串聯式質譜儀, 紅酒, 定量, Resveratrol, QuEChERS, HPLC-MS/MS, red wine, quantitation