摘要
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1～300μg/L,相关系数为0.998 5.MSPD法回收率大于90%,检出限为0.3μg/kg;SPE法回收率大于80%,检出限为0.5μg/kg.2种方法均满足残留分析的要求.将2种前处理方法的步骤与结果进行比较,MSPD法萃取水产品中DES的残留更简便、省时以及更节省溶剂.
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.
出处
《分析测试技术与仪器》
CAS
2011年第4期211-216,共6页
Analysis and Testing Technology and Instruments
基金
中国水产科学研究院院部中央级公益性科研院所基本科研业务费专项(2011C008)
作者简介
尹怡（1982-），女，助理研究员，主要从事水产品质量安全检测工作．Tel：020—81616509．E—mail：yin．yi@126．com
通讯作者：朱新平，男，研究员，博士生导师．Email：zhuxinping_1964@yahoo．com．cn
