加速溶剂萃取/气相色谱质谱法测定鱼类样品中的多环麝香

建立了鱼类样品中5种多环麝香的分析方法.采用加速溶剂萃取(ASE)提取,经凝胶渗透色谱(GPC)以及中性氧化铝层析柱净化后,浓缩并定容洗脱液,用GC-SIM-MS进行检测.本方法对替代物标样荧蒽-d10的回收率为92.7%—112.9%.以六氯苯(13C)为内标,5种合成麝香的线性范围为1.0—1000.0 n.gg-1.麝香的检出限为0.20—0.30 n.gg-1(S/N=3).5种化合物的基质加标回收实验的平均回收率为89.6%—110.1%,RSD为3.2%—8.8%.方法准确,可用于实际样品的检测.

鱼类样品中有机磷阻燃剂分析方法的优化研究

建立了鱼类组织样品中有机磷阻燃剂(OPFRs)的分析方法,优化了萃取条件、净化条件、液相色谱条件和质谱检测参数。确定了生物样品经冷冻干燥后,以1∶1(V/V)的正己烷/二氯甲烷混合溶液进行加速溶剂萃取,利用氨基固相萃取柱进行净化,以1∶1(V/V)的正己烷/二氯甲烷、二氯甲烷和9∶1(V/V)的二氯甲烷/甲醇为洗脱液,最后用超高效液相色谱-串联质谱同时对9种OPFRs进行定性定量检测。结果表明,各物质的基质加标回收率均为56.5%~108%,方法的测定下限为0.016~0.104 ng/g(以脂重计),满足了生物样品中OPFRs的分析检测要求。利用该方法测定了北京和广州市养殖和野生鲫鱼肌肉组织样品,主要的OPFRs同族体为磷酸三正丁酯(TNBP)、磷酸三乙基己基酯(TEHP)、磷酸三(1-氯-2-丙基)酯(TCIPP)和磷酸三氯乙基酯(TCEP),质量比为5.94~33.7 ng/g(以脂重计),显示出良好的适用性。

An Investigation of Elements （Mercury） Status in Marshes in South of Iraq

The study was conducted to investigate the mercury status in three major marshes in southeast Iraq. Sediments, plants （three species） and fish （five species） samples were collected at five locations along the major marshes （AL-Hammar, Cross of AI Fuhod AI Tar, Downstream of AL-Mashab ＆ AL-Salal, Hawizeh and AL-Chebayesh） in southeast Iraq and analysed for mercury concentrations. The sediments were collected at predetermined input and output sources. The mercury concentrations were extremely high in both the sediment and plant samples but variable in fish species. There was a strong relationship between mercury concentrations in the sediments and fishes. Some of the fish species have mercury levels that are considered safe by the international marketing standard/WHO recommendation while others contain mercury levels that may be considered unsafe for human consumption.