QuEChERS-气相色谱质谱测定谷物中16种欧盟优控多环芳烃

Determination of 16 European Union-controlled polycyclic aromatic hydrocarbons in cereals by gas chromatography-mass spectrometry combined with QuEChERS

目的建立谷物中16种欧盟优控多环芳烃(European Union priority controlled polycyclic aromatic hydrocarbons,EUPAHs)的快捷、简便、廉价、有效、可靠、安全的样品前处理(quick、easy、cheap、effective、rugged、safe,QuEChERS)-气相色谱质谱(gas chromatograph-mass spectrometer,GC-MS)检测方法。方法样品经10 mL正己烷超声提取后,取上清液用N-丙基乙二胺(PSA)粉末和无水硫酸镁净化,净化液于35℃下氮气缓慢浓缩至近干,加入1 mL丙酮-异辛烷(1∶1,V/V),过0.22μm有机膜,用GC-MS进行测定。结果16种EUPAHs在10~300 ng/mL的线性范围内,所得回归方程均呈良好的线性关系,相关系数在0.9988~0.9997之间;方法检出限为0.1~8.0μg/kg,方法定量限为0.3~25.0μg/kg;平均回收率为68.4%~114.8%,相对标准偏差为2.8%~11.6%。结论所建立的方法灵敏度高,定量准确,操作简便,适用于谷物中16种EUPAHs的检测。

Objective To establish a quick,easy,cheap,effective,rugged and safe sample pretreatment(QuEChERS)-gas chromatography mass spectrometry(GC-MS)detection method for 16 European Union priority controlled polycyclic aromatic hydrocarbons(EUPAHs)in cereals.Methods After the samples were treated by ultrasonic extraction with 10 mL n-hexane,the supernatant was purified with primary secondary amine(PSA)powder and anhydrous magnesium sulfate,and the purified liquid was slowly concentrated to near dryness under nitrogen at 35℃,and measured by GC-MS after adding 1 mL of acetone isooctane(1∶1,V/V)and filtering over 0.22μm organic membrane.Results In the linear range of 10-300 ng/mL,the regression equations of 16 kinds of EUPAHs showed a good linear relationship,the correlation coefficients were 0.9988-0.9997.The detection limit was 0.1-8.0μg/kg,the lower limit of quantification was 0.3-25.0μg/kg,the average recoveries were 68.4%-114.8%,and the relative standard deviations were 2.8%-11.6%.Conclusion This method is highly sensitive,quantitatively accurate and easy to operate,and is suitable for the detection of 16 EUPAHs in cereals.