固相萃取-高效液相色谱法测定纺织品中富马酸二甲酯

Determination of dimethyl fumarate in textiles by solid phase extraction-high-performance liquid chromatography

建立了纺织品中富马酸二甲酯的固相萃取-高效液相色谱检测方法.样品经超声提取后,采用固相萃取净化,Kromasil C18柱（250 mm×4.6 mmi.d.,5μm）分离,采用乙腈/水（体积比为55/45）为流动相,紫外检测波长为220 nm,外标法定量.结果表明：富马酸二甲酯在0.05～ 50.0 mg/L的浓度范围内呈良好的线性关系,最低检出限LOD为0.02 mg/kg,定量检出限LOQ为0.05 mg/kg,回收率在91.2％ ～102.1％之间,平均回收率为96.4％,RSD为1.3％ ～3.9％.所建实验方法快速、简便、干扰少,能满足纺织品中富马酸二甲酯的测定要求.

To establish a method for the determination of dimethyl fumarate in textiles by solid phase extraction-high performance liquid chromatography, samples were ultrasonic extracted, cleaned and enriched by a Sep-Pak Vac Silica solid-phase extraction（SPE） cartridge, and separated on a Kromasil C18 column （250 mm × 4.6 mm i. d., 5 um ）by using the mobile phase consisting of CHaCN ＋ H2O （55/45, V/V）. Detection was performed at the wavelength 220 nm using extenal standard method. The result of experiment showed that calibration curve of dimethyl fumarate was linear within the range of 0.05 - 50.0 mg/L, the limit of detection was found to be 0.02 mg/kg, and the limit of quantification was be found to be 0.05 mg/kg. The extraction recoveries were at 91.2% - 102. 1% ,average recovery was 96.4% and the RSDs were at 1.3% -3.9%. The developed method is quick,simple and little interferential for the determination of dimethyl fumarate residue in textiles.