摘要
建立了水产品中7种多氯联苯残留的气相色谱检测方法。采用HP-5石英毛细管柱(30 m×0.32 mm×0.25μm)以及气相色谱仪(带电子捕获检测器)在程序升温的条件下分离水产品中7种多氯联苯残留。方法线性范围为1~180 ng/mL,相关系数均大于0.999,定量限为0.5μg/kg,检测限为0.3μg/kg。该方法采用正己烷/二氯甲烷(9∶1)提取,佛罗里硅土分散固相萃取、净化,结果准确可靠,重复性好,回收率为84.7%~112%,相对标准偏差为0.79%~8.88%,可满足实验室对水产品中7种多氯联苯快速分析的需要。
A method for determining residues of seven kinds of polychlorinated biphenyls in aquatic products by gas chromatography was developed. The reconstituted sample was transferred to GC - ECD for detection using the HP - 5 silica capillary chromatograph column ( 30 m × 0. 32 mm × 0. 25 um ), and the seven kinds of polychlorinated biphenyls in aquatic products were separated with the oven program. The test results showed that the method was linear within the range assayed of 1 - 180 ng/mL, all correlation coefficients were over O. 999, the limit of quantification(LOQ) was 0. 5 ug/kg, the limit of detection(LOD) was 0.3 ug/kg. The analytes were extracted with blended solution of hexane and dichloromethane (9 : 1 ), Florisil dispersive solid - phase extraction cleaned up. And the results had nicety and good repetition with the average recoveries ranging from 84.7% to 112% and the relative standard deviations from 0.79% -8.88%.
出处
《中国兽药杂志》
2011年第6期22-25,52,共5页
Chinese Journal of Veterinary Drug
关键词
基质固相分散萃取
多氯联苯
气相色谱
水产品
matrix solid - phase dispersion ( MSPD )
polychlorinated biphenyls
gas chromatography
aquatic products