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目的建立金枪鱼中7种指示性多氯联苯的三重四级杆气相色谱分析方法。方法金枪鱼采用经典的索氏提取法,以PCB198为定量内标,使用正己烷-二氯甲烷(1∶1,V/V)混合溶液作为提取溶液,提取液经浓缩后用固相萃取柱净化,经DB-5MS色谱柱程序升温分离,采用Acquisition-Timed方法,SRM扫描。结果 7种多氯联苯的质量浓度在10.0μg/L~400.0μg/L呈良好的线性关系,相关系数r为0.996 9~0.999 3,平均回收率为80.0%~114.0%,相对标准偏差(RSD)为1.98%~3.89%,方法检出限为0.02μg/kg~0.10μg/kg。结论本方法简单、快速、可靠,通过二级质谱扫描,减少了在复杂基质样品中的背景干扰,提高了目标化合物的检测灵敏度。
Objective To establish a triple quadrupole gas chromatographic method for the determination of 7 indicative polychlorinated biphenyls (PCBs) in tuna. Methods The classic Soxhlet extraction method was used to determine the amount of PCB198 in the tuna. The n-hexane-dichloromethane (1: 1, V / V) mixed solution was used as the extraction solution. , The temperature was separated by DB-5MS column chromatography, using Acquisition-Timed method, SRM scanning. Results The concentrations of seven PCBs showed a good linearity between 10.0μg / L and 400.0μg / L with a correlation coefficient of 0.996 9 to 0.999 3 and an average recovery of 80.0% to 114.0%. The relative standard deviations RSD) ranged from 1.98% to 3.89%. The detection limits were 0.02μg / kg ~ 0.10μg / kg. Conclusion The method is simple, rapid and reliable. By the second-order MS scan, the background interference in complex matrix samples is reduced and the detection sensitivity of the target compounds is improved.