SPE-UHPLC测定淀粉及淀粉制品中丁烯二酸类酸度调节剂

Determination of Maleic Acid and Fumaric Acid in Starch and Starch Products Using SPE-UHPLC Method

建立固相萃取-超高效液相色谱法测定淀粉及淀粉制品中的顺丁烯二酸、顺丁烯二酸酐和反丁烯二酸含量的检测方法.样品经ProElut PWA混合型弱阴离子交换固相萃取柱净化,超高效液相色谱分析,采用Waters Acquity UPLC HSS T3色谱柱,洗脱液为φ（磷酸）=0.10％水溶液与甲醇的体积比为98：2,检测波长214 nm,流速0.2 mL·min-1.在此条件下,顺反丁烯二酸分离良好且无杂质峰干扰,样品加标回收率83.81％ ～ 108.03％,相对标准偏差（n=8）小于10％,顺丁烯二酸和反丁烯二酸的定量限为0.25 mg·kg-1,能够满足实际检测需要.

In the present study, a solid-phase extraction ultra high performance liquid chromatographic （UHPLC） method was established for the analysis of maleic acid, fumaric acid, and maleic anhydride in starch and starch products. Starch samples were cleaned up by ProElut PWA mixed-mode weak anion ex- changer SPE columns. Waters Acquity UPLC HSS T3 was used for chromatographic separation and the separation condition was 0. 10% phosphoric acid aqueous solution and methanol （98： 2, V/V） , detection wavelength 214 nm, and flow rate 0.2 mL.min-1. The average spiked recoveries were in the range of 83.81% and 108.03% with RSDs （n =8） less than 10% and the LOQs of maleic acid and fumaric acid were 0.25 rng.kg-1. The method could satisfy with the requirement for the determination of maleic acid and fumaric acid in actual samples.