基质固相分散法与固相萃取法在检测水产品中己烯雌酚残留中的应用

分别建立了基质固相分散（MSPD）法、固相萃取（SPE）法与气相色谱/质谱联用（GC-MS）测定水产品中己烯雌酚（DES）残留量的分析方法，并对MSPD与SPE 2种样品前处理方法的效果进行了比较。MSPD法中样品以弗罗里硅土（Florisil）作为固相分散剂，经乙酸乙酯提取，再用Florisil净化；SPE法中样品经乙酸乙酯超声提取，过Florisil小柱进行净化，最后经GC-MS在选择离子监测模式下测定水产品中DES。在优化的色谱条件下，方法的线性范围为1-300 μg/L，相关系数为0.9985。M

Comparison of Matrix Solid Phase Dispersion and Solid Phase Extraction in Analysis of Diethylstilbestrol Residue in Aquatic Products

The matrix solid phase dispersion（MSPD）and solid phase extraction（SPE）coupled with gas chromatography-mass spectrometry（GC-MS） methods have been established for the determination of diethylstilbestrol（DES）in aquatic products.DES was extracted with ethyl acetate and cleaned up by the dispersive method with Florisil,whereas,ultrasonic extraction with ethyl acetate and Florisil SPE column purification were employed in the SPE analytical procedure.DES in the extracts were then quantified by GC-MS.Good linear range（r2=0.9985） between 1~300μg/L was obtained under the optimized chromatographic conditions.Comparing the recovery（80%） and LOD（0.5 μg /kg） with SPE method,MSPD has a higher recovery（90%） and a lower LOD（0.3 μg /kg）.Both these methods fulfill the requirements of the analysis of residues.Through the comparison of analytical procedure and results,it is confirmed that the MSPD method is quicker and simpler than the SPE method.