摘要
建立测定糕点食品中9种Amadori化合物的液相色谱-串联质谱(LC-MS/MS)方法。样品经甲醇萃取、正己烷除脂,经QuEChERS(50 mg PSA和100 mg C18混合物)净化后,进行LC-MS/MS测定分析。流动相为甲醇与0.5%甲酸水溶液,用Waters Acquity BEH C18(100 mm×2.1 mm,1.7μm)分离。结果表明:该方法检出限在0.13~0.70μg/g,日内精密度RSD(n=6)在2.44%~5.79%,日间精密度RSD(n=3)在3.02%~5.97%,稳定性好,回收率在80.3%~112.4%,准确性高。该方法准确可靠、灵敏度高,非常适合复杂基质糕点类食品中9种Amadori化合物的分析。
A rapid method for simultaneously determining 9 Amadori compounds in pastry food by high performance liquid chromatography-triple quaternary mass spectrometry was developed. The pastry food was extracted with methanol, n-hexane degreased, and purified by QuEChERS(50 mg PSA and 100 mg C18 mixture), then analyzed by LC-MS/MS. The samples were separated on an Waters Acquity BEH C18 column with the gradient elution mobile phase of methanol and 0.5%(v/v) formic acid aqueous solution. Results showed that: the limit of detection was between 0.13 μg/kg and 0.70 μg/kg, the intra-day and the inter-day relative standard deviations(RSDs) were 2.44%~5.79%(n=6) and 3.02%~5.97%(n=3), the standard recoveries of the spiked samples ranged from 80.3% to 112.4%. The method was accurate, reliable and sensitive, and was very suitable for the analysis of the 9 Amadori compounds in pastry food.
引文
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