Carb/NH2固相萃取结合气相色谱-质谱法测定兰州百合中16种多环芳烃

Determination of 16 Polycyclic Aromatic Hydrocarbons in Lilium davidii var.unicolor by Carb/NH2 Solid Phase Extraction Combined with Gas Chromatography-Mass Spectrometry

通过优化前处理条件建立了基于气相色谱-质谱联用仪(GC-MS)检测兰州百合中16种多环芳烃(PAHs)的方法.样品中加水充分浸润,用乙腈提取,加硫酸镁和氯化钠混合粉末进行除水,涡旋提取后浓缩至2 mL,用Carb/NH2固相萃取柱净化,正己烷溶解,DB-5MS毛细管柱(Agilent,30 m×250µm,0.25µm)分离,GC-MS分析,外标法定量.测得的16种PAHs的相关系数均大于0.99,检出限范围为0.2~0.8µg/kg,定量限范围为0.9~3.1µg/kg,相对标准偏差为1.75%~5.14%.建立的方法稳定、灵敏、准确,可用于兰州百合样品中PAHs的日常监督检测.

By optimizing the pretreatment conditions,a method for the determination of 16 polycyclic aromatic hydrocarbons(PAHs)in Lilium davidii var.unicolor by gas chromatography-mass spectrometry(GC-MS)has been established.The samples were infiltrated with deionized water,extracted with acetonitrile,and dehydrated with mixed powder of MgSO4 and NaCl.After extraction,the samples were concentrated to 2 mL.The samples were purified by a Carb/NH2 solid phase extraction column,dissolved in n-hexane,separated by a DB-5MS capillary column(Agilent,30 m×250μm,0.25μm),analyzed by GC-MS,and quantified by external standard method.The correlation coefficients of 16 PAHs were all greater than 0.99,the limits of detection were 0.2~0.8μg/kg,the limits of quantification were 0.9~3.1μg/kg,and the relative standard deviations were 1.75%~5.14%.The method is reliable,sensitive and accurate,and can be used for daily monitoring and detection of PAHs in the Lilium davidii var.unicolor.