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目的建立乳饮料、碳酸饮料和茶饮料等3种常见饮料中富马酸二甲酯的分散固相萃取-高效液相色谱测定方法。方法样品经甲酸酸化后,用PSA吸附剂进行净化,在Kromasil C18(250 mm×4.6 mm i.d.,5μm)色谱柱上,以乙腈/水(55/45,V/V)为流动相进行分离,紫外220 nm检测,外标法定量。结果在酸性条件下,PSA相比C18、PRS和WCX等吸附剂能更有效地吸附饮料基质中的脂肪酸、有机酸、色素以及糖类等物质,其最佳条件为2.0 g饮料中加入30μl甲酸和100 mg PSA。富马酸二甲酯在0.1 mg/L~10.0 mg/L范围内具有良好的线性,相关系数为0.9995,回收率在86.0%~102.0%范围,相对标准偏差(RSD)在0.6%~6.3%之间,最低定量检出限为0.1 mg/kg范围。结论建立的分散固相萃取-高效液相色谱测定方法具有简便、快速、干扰少等特点,适合于饮料中富马酸二甲酯的快速检测。
OBJECTIVE To establish a method for the determination of dimethyl fumarate in milk, carbonated drinks and tea beverages by dispersive solid-phase extraction-high performance liquid chromatography. Methods The sample was acidified with formic acid and purified with PSA adsorbent. The sample was separated on a Kromasil C18 (250 mm × 4.6 mm id, 5 μm) column with acetonitrile / water (55/45, V / V) UV 220 nm detection, external standard quantitative. Results Compared with C18, PRS and WCX adsorbents, PSA could adsorb fatty acids, organic acids, pigments and carbohydrates in the beverage matrix more effectively under the acidic conditions. The optimal conditions for the PSA were 2.0 g of beverage, 30 μl of formic acid And 100 mg PSA. Dimethyl fumarate showed a good linearity in the range of 0.1 mg / L ~ 10.0 mg / L, the correlation coefficient was 0.9995, the recoveries ranged from 86.0% to 102.0%, and the relative standard deviations (RSDs) ranged from 0.6% to 6.3% The lowest limit of quantification was 0.1 mg / kg. Conclusion The established dispersive solid phase extraction - high performance liquid chromatography has the advantages of simple, rapid, less interference and is suitable for the rapid detection of dimethyl fumarate in beverages.