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建立了固相萃取-超高效液相色谱(UPLC)同时测定乳制品中苹果酸、酒石酸、乳酸、乙酸、柠檬酸、富马酸等6种有机酸的分析方法。样品用体积分数1%氨水溶液提取,调节至中性后经MAX柱净化,用Acquity UPLC HSS T3色谱柱(2.1 mm×100 mm,1.8μm)分离,以乙腈和0.02 mol/L KH2PO4缓冲溶液(pH 2.0)作为流动相进行梯度洗脱,二极管阵列检测器检测。6种有机酸在其相应范围内(0.05~5000 mg/L)线性关系良好(r2≥0.999),方法的定量限(信噪比为10)为0.05~25.0 mg/kg,3个不同水平的添加浓度回收率为80.1%~103.2%,相对标准偏差(n=8)在1.9%~11%之间。方法适合于乳制品中6种有机酸的同时检测。
A method for simultaneous determination of six organic acids, including malic acid, tartaric acid, lactic acid, acetic acid, citric acid and fumaric acid, in dairy products by solid phase extraction coupled with ultra performance liquid chromatography (UPLC) was established. The sample was extracted with 1% ammonia solution and adjusted to neutrality. The sample was purified by MAX column and separated on an Acquity UPLC HSS T3 column (2.1 mm × 100 mm, 1.8 μm). The sample was eluted with acetonitrile and 0.02 mol / L KH2PO4 buffer solution pH 2.0) as mobile phase gradient elution, diode array detector detection. The linear range of the six organic acids was within the range of 0.05-5000 mg / L (r2≥0.999). The limit of quantification (S / N ratio) of the six organic acids ranged from 0.05 to 25.0 mg / kg with three different levels The recoveries were 80.1% ~ 103.2%, and the relative standard deviations (n = 8) ranged from 1.9% to 11%. The method is suitable for the simultaneous detection of six organic acids in dairy products.