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目的建立用高效液相色谱法同时测定面制品中的顺丁烯二酸和富马酸含量。方法样品经50 ml 10%甲醇-水萃取,离心后,水层过0.45μm滤膜,经Waters Atlantis T3色谱柱(250 mm×4.6 mm,5μm)分离,以0.1%磷酸-甲醇(95∶5,V/V)作流动相,紫外检测器检测,波长210 nm。结果在优化的试验条件下,顺丁烯二酸和富马酸的浓度在0.1~25μg/ml范围内与峰面积呈良好的线性关系,回归方程分别为y_(顺丁烯二酸)=147008x-1316.8(r=0.999 5,n=6)和y_(富马酸)=176689x-670.1(r=0.999 6,n=6),方法检出限均为2.0 mg/kg,回收率为86.88%~93.02%,相对标准偏差为0.67%~1.08%。结论该方法简便、准确,可适用于面制品中顺丁烯二酸和富马酸的同时测定。
Objective To establish simultaneous determination of maleic acid and fumaric acid in flour products by high performance liquid chromatography. Methods The samples were extracted with 50 ml of 10% methanol-water. After centrifugation, the aqueous layer was filtered through a 0.45 μm membrane and separated on a Waters Atlantis T3 column (250 mm × 4.6 mm, 5 μm) with 0.1% phosphoric acid- , V / V) as the mobile phase, UV detector detection, wavelength 210 nm. Results Under the optimum conditions, the concentration of maleic acid and fumaric acid showed a good linear relationship with the peak area in the range of 0.1 ~ 25μg / ml. The regression equation was y_ (maleic acid) = 147008x -1316.8 (r = 0.999 5, n = 6) and y_ (fumaric acid) = 176689x-670.1 (r = 0.999 6, n = 6). The detection limits were both 2.0 mg / kg and the recoveries were 86.88% ~ 93.02%, the relative standard deviation was 0.67% ~ 1.08%. Conclusion The method is simple and accurate and can be applied to the simultaneous determination of maleic acid and fumaric acid in flour products.