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建立中空纤维液相微萃取(HF-LPME)-高效液相色谱(HPLC)测定复杂样品中顺/反丁烯二酸含量的新方法。分别对萃取溶剂、样品p H值、萃取温度、萃取时间、搅拌速率以及盐浓度等LPME参数进行了优化,确定最佳优化条件为:以磷酸三丁酯为萃取剂,样品p H值为0.9,温度为20℃,萃取时间为40 min,搅拌速率为500 r/min,不添加盐。结果在最优化的条件下,顺丁烯二酸在(0.1~10.0)mg/L范围内线性关系良好,相关系数大于0.999,相对标准偏差为1.7%(n=11),检出限LOD为5.12μg/L,富集倍数可达12.9;反丁烯二酸在(0.01~1.0)mg/L范围内线性关系良好,相关系数大于0.999,相对标准偏差为4.3%(n=11),检出限LOD为1.28μg/L,富集倍数可达46.2倍。将以上所建立的方法用于淀粉样品中顺/反丁烯二酸的测定研究,加标回收率和精密度均满足分析方法的要求,实现了实际样品中顺/反丁烯二酸的准确灵敏检测。
A new method for determination of cis / 2-fumaric acid in complex samples by hollow fiber liquid-phase microextraction (HF-LPME) and high performance liquid chromatography (HPLC) was established. LPME parameters such as extraction solvent, p H value, extraction temperature, extraction time, stirring rate and salt concentration were optimized respectively. The optimum conditions were as follows: p-value of 0.9 , The temperature was 20 ℃, the extraction time was 40 min, the stirring rate was 500 r / min, no salt was added. Results Under the optimal conditions, the linearity of maleic acid in the range of (0.1-10.0) mg / L was good with the correlation coefficient greater than 0.999 and the relative standard deviation of 1.7% (n = 11). The LOD was 5.12μg / L, enrichment multiple of up to 12.9; fumaric acid in the (0.01 ~ 1.0) mg / L range of good linear correlation coefficient greater than 0.999, the relative standard deviation of 4.3% (n = 11) The limit LOD was 1.28μg / L, the enrichment factor can reach 46.2 times. The method established above was applied to the determination of cis / fumaric acid in starch samples. The spiked recoveries and precision met the requirements of the analytical method and the accuracy of cis / fumaric acid in the actual samples was achieved Sensitive detection.