Page B D, Lacroix G
Health and Welfare Canada, Health Protection Branch, Ottawa, Ontario.
J Chromatogr. 1993 Oct 1;648(1):199-211. doi: 10.1016/0021-9673(93)83303-a.
Solid-phase microextraction (SPME), with the poly(dimethylsiloxane)-coated silica fiber suspended and equilibrated in the headspace, has been applied to the capillary gas chromatographic (GC) analysis of 33 halogenated volatile contaminants in model aqueous solutions and in foods. With electrolytic conductivity detection, the limits of detection in water ranged from 1.5 micrograms/kg for vinyl chloride to < or = 0.005 microgram/kg for the tri- to hexachlorobenzenes. Headspace SPME-GC shows a much greater response for the less volatile analytes than those of greater volatility, a procedure complementing headspace GC with gas sampling. In model systems or foods, increasing lipid material decreased the headspace extraction. With 50 mg of lipid, the headspace extraction decreased about 50% for analytes with LODs about 0.1 microgram/kg and by > or = 99.5% for the above chlorobenzenes. Standard addition was used to analyze a variety of beverages and dry foods and to determine the analyte partitions.
将涂有聚二甲基硅氧烷的石英纤维悬浮并在顶空中平衡的固相微萃取（SPME）已应用于对模拟水溶液和食品中33种卤代挥发性污染物的毛细管气相色谱（GC）分析。采用电解电导检测，水中的检测限范围为氯乙烯的1.5微克/千克至三氯苯至六氯苯的≤0.005微克/千克。顶空固相微萃取-气相色谱对挥发性较低的分析物的响应比对挥发性较高的分析物大得多，该方法是对顶空气相色谱与气体采样的补充。在模型系统或食品中，增加脂质物质会降低顶空萃取。对于50毫克脂质，对于检测限约为0.1微克/千克的分析物，顶空萃取降低约50%，对于上述氯苯则降低≥99.5%。采用标准加入法分析了多种饮料和干燥食品，并确定了分析物的分配情况。
