CAJ | 학술논문

目的：建立食品样品中P26, P50, P62等三大指示性毒杀芬的检测分析方法,为进一步开展常规监测提供技术平台和基础数据。方法食品样品使用索式提取系统(Soxtec)提取,提取液依次由30%酸性硅胶柱和氧化铝柱净化,利用同位素稀释-高分辨气相色谱/高分辨双聚焦磁式质谱联用(ID-HRGC/HRMS)技术对三种指示性毒杀芬单体P26, P50, P62进行定量定性分析。结果本研究所建成的检测方法相对标准偏差(RSD)小于25%,回收率可以达到40%~120%；P26, P50, P62的方法检测限分别为0.08、0.02、0.06 pg/g；方法性能达到开展食品样品中毒杀芬检测技术的要求。结论该方法可以对食品样品中毒杀芬进行检测,检测效率高,结果准确可靠。
목적：건립식품양품중P26, P50, P62등삼대지시성독살분적검측분석방법,위진일보개전상규감측제공기술평태화기출수거。방법식품양품사용색식제취계통(Soxtec)제취,제취액의차유30%산성규효주화양화려주정화,이용동위소희석-고분변기상색보/고분변쌍취초자식질보련용(ID-HRGC/HRMS)기술대삼충지시성독살분단체P26, P50, P62진행정량정성분석。결과본연구소건성적검측방법상대표준편차(RSD)소우25%,회수솔가이체도40%~120%；P26, P50, P62적방법검측한분별위0.08、0.02、0.06 pg/g；방법성능체도개전식품양품중독살분검측기술적요구。결론해방법가이대식품양품중독살분진행검측,검측효솔고,결과준학가고。
Objectives To develop the analyzing methods of 3 indicator toxaphenes (P26, P50 and P62) in food samples, so as to provide technical platform and basic data for further routine monitoring. Methods The food sample was extracted by using Soxtec followed by purification on 30%multilayer acidic silica column and neutral aluminum oxides column, utilizing isotope dilution high-resolution gas chromatography/high-resolution double-focusing magnetic mass spectrometry (HRGC/HRMS) to carry out quantitative and qualitative analysis on toxaphene monomer P26, P50, and P62. Results The developed analytical method for three indicator tox-aphenes monomer was built successfully, and suitable for the determination of toxaphene specific congeners in food. The relative standard deviation (RSD) was below 25% and the spiked recoveries were in the range of 40%~120%. The five point calibration curves showed a good linearity for all the congeners (R2>0.99). Method detection limit (MDL) was 0.08, 0.02, and 0.06 pg/g for P26, P50, and P62, respectively. Conclusion Three congeners of toxaphene can be measured simultaneously in food sample matrix, the method is efficient and the results are accurate and reliable.