摘要
应用气相色谱法与顶空固相微萃取样品预处理技术相结合的方法,测定水产品中五氯酚（PCP）。选用20 m L顶空瓶,其中预置1 mol/L盐酸溶液0.7 m L及氯化钠4.0 g,加入1.0 g样品用1 mol/L氢氧化钠溶液定容10 m L,立即封盖。插入85μm聚丙烯酸醋萃取头于65℃平衡35 min后的顶空瓶萃取15 min,随之进入色谱仪解吸3 min并测定。测定中采用HP-5毛细管柱和程序升温（40℃~280℃）条件,并用载气流量为3 m L/min。测得五氯酚（PCP）的方法定量限为0.15μg/kg,标准曲线的相关系数为0.995,样品低、中、高三种浓度的加标后回收率为96.3%~112.6%,相对标准偏差（n=6）为3.3%~4.5%。该法快速、准确、绿色、无污染的检测出水产品中五氯酚的残留量的方法技术,并应用于日常监测与检测中,最终杜绝食品安全隐患问题。
Study the method for determination ofchlomphenols in aquatic products by using headspace solid phase microextraction and gas chromatography. The homogenized sample was extracted ultrasonically at 40 ℃ for 30 min in a solution containing 4.0 g of NaCl and 0.7 mL of HCl solution in a 20 mL headspace bottle, which was constant volume 10 mL by 1 mol/L NaOH, then sealed it. Heat at 65 ℃ for 35min and separated by SPME for 15 min, with the 85 tam PA extractor. After pyrolysis from 40℃ to 280℃ with 3 mL/min airflow, and separation on HP-5 capillary column, content of pentachlomphenol （PCP） was determined by GC with ECD. Linearity range of mass concentration of PCP was found to be 0.995, and the detection limit （3S/N） was found to be 0.15 μg/ kg. Recovery was tested at 3 concentration levels, in the range of 96.3%~112.6%, and RSD （n=6） ranged from 3.3% to 4.5%. The green, pollution-free, quickly and accurately detection method ofpentachlomphenol residues in aquatic products technology, applied to routine monitoring and testing, to put an end to food safety concems.
出处
《食品工业》
北大核心
2015年第1期271-274,共4页
The Food Industry
基金
辽宁省质量监督局科技计划项目专项基金
关键词
气相色谱法
顶空固相微萃取
五氯酚
水产品
gas chromatography
pheadspace solid phase microextraction
chlorophenols
aquatic products
