固相萃取-气相色谱联用测定海洋沉积物中的长链烯酮

Determination of Long-chain Alkenones in Marine Sediments Using SPE-GC Method

建立了测定痕量长链烯酮的分析方法,获得了优化的前处理条件、气相色谱检测条件。对定性定量方法及实验条件必须满足的要求进行了评价。通过过程质量控制(Quality Control,QC)对整个方法进行了验证。结果显示,本研究所建立的分析方法能够满足沉积物样品长链烯酮测定的要求:仪器的检测限分别为25.75ng/g和28.54ng/g;方法的检测限分别为86ng/g和95ng/g;平均回收率介于67%～89%,回收率相对标准偏差分别为9.33%和9.39%;精密度RSD(C37∶3)=14.07%,RSD(C37∶2)=13.17%。利用此方法对部分样品进行了分析,测得的结果与布莱梅大学实验室所测的一致。

The study aim is to build a method of determining long- chain alkenones in marine sediments, and to gain the optimum condition of preparation of samples, and the best condition of Gas Chromatogra- phy （GC） and to assess, the requirement of quality, quantity and experimental condition. According to the validation of the quality control （QC）, the results proved that the analytical method satisfied the require- ments of the determination of long- chain alkenones in marine sediments. The instrument limits of detec- tion were LOD（C37：3）=25. 75 ng/g, LOD（Car,z）= 28. 54 ng/g; the method limits of detection were LOD （C37：3）=86 ng/g,LOD（C37：2）=95 ng/g . and the recoveries were between 67%~89%, of which the rela- tive standard deviations were 9.33% ,9.39%. RSD（C37,a）= 14.07%,RSD（C37：2）--13. 17%. Based on the determination method, several samples were analyzed and have the same results which analyzed in different lab.