固相萃取/气相色谱-串联质谱法测定竹笋产地土壤中42种持久性有机污染物

Determination of 42 Persistent Organic Pollutants in Geographical Original Soil of Bamboo Shoot by Gas Chromatography-Tandem Mass Spectrometry with Solid Phase Extraction

建立了同时测定竹笋产地土壤中8种多环芳烃(PAHs)、18种多氯联苯(PCBs)和16种有机氯农药(OCPs)的方法。样品经丙酮-正己烷(1∶1,体积比)大功率超声提取,复合弗罗里硅土柱固相萃取净化、氮吹浓缩后,利用气相色谱-三重四极杆质谱(GC-MS/MS)测定。结果表明,42种持久性有机污染物(POPs)在35 min内得到分离,在2. 0～2 000. 0μg/L范围内线性关系良好,相关系数(r2)为0. 995 2～0. 999 8;方法的加标回收率为62. 3%～128%,相对标准偏差(RSD)为0. 5%～15. 8%,检出限(S/N=3)为0. 070～6. 902μg/kg。该法操作简便,准确度好,灵敏度高,可用于竹笋产地土壤样品中42种POPs的同时测定。

A method of gas chromatography-tandem mass spectrometry(GC-MS/MS)was developed for the determination of 8 polyaromatic hydrocarbons(PAHs),18 polychlorinated biphenyls(PCBs)and 16 organochlorine pesticides(OCPs)in geographical original soil of bamboo shoot.The samples were extracted with acetone-hexane(1∶1,by volume)in an superpower ultrasonic bath,then purified with a Florisil composite column.The eluant was concentrated by N 2 blowing,finally detemined by GC-MS/MS.42 persistent organic pollutants(POPs)were efficiently separated within 35 min,and there were good linearities for the analytes in the concentration range of 2.0-2 000.0μg/L with their correlation coefficients(r^2)of 0.995 2-0.999 8.The spiked recoveries ranged from 62.3%to 128%with relative standard deviations of 0.5%-15.8%,and the limits of detection(S/N=3)were 0.070-6.902μg/kg.With the characteristics of easy operation,high sensitivity and accuracy,the method could be applied in the simultaneous detection of 42 POPs in original soil of bamboo shoot.