基于固相萃取技术的液相色谱-串联质谱法快速检测食用油脂中的苯并(a)芘  

Study on the Application of Liquid Chromatography-Tandem Mass Spectrometry Based on Solid Phase Extraction Technique for Rapid Detection of Benzo(a) Pyrene in Edible Oils and Fats

作　　者：郭芳芳[1] 王明明[1] 王果 彭雪琦 葛晓晓 舒蕊华 GUO Fangfang;WANG Mingming;WANG Guo;PENG Xueqi;GE Xiaoxiao;SHU Ruihua(Jiangsu Physical and Chemical Testing Center,Nanjing 210000,China)

机构地区：[1]江苏省理化测试中心,江苏南京210000

出　　处：《食品科技》2020年第8期271-275,共5页Food Science and Technology

摘　　要：以键合硅胶的C18填料和弗罗里硅土填料分层装填的复合固相萃取柱为净化技术,建立一种液相色谱-串联质谱(LC-MS/MS)快速检测食用油脂中苯并(a)芘的分析方法。食用油脂无需溶剂提取,直接进入固相萃取柱,乙腈洗脱,氮吹浓缩定容后经液相色谱-联质谱仪检测,内标法定量。考察了固相萃取柱填料类型、填料用量、洗脱溶剂、洗脱体积等因素对提取效率的影响。在优化的条件下,苯并(a)芘线性范围为0.5~10.0 ng/mL,相关系数≥0.999,检出限为0.1 μg/kg,定量限为0.4 μg/kg。样品在0.4、1.0、10.0 μg/kg 3个水平下的加标回收率为77.5%~94.8%,相对标准偏差为0.65%~4.72%。该法操作简便、快速、准确度高,检出限能满足食用油脂中苯并(a)芘残留的检测要求,分析成本低,可为其他产品中的苯并(a)芘测定提供参考。The composite solid phase extraction column with bonded silica gel C18 packing and florey silica soil packing layered filling was used as the purification skill,to establish a method of rapid determination of benzo (a) pyrene in edible oils by liquid chromatography-tandem mass spectrometry (LC-MS/MS).The edible oils and fats did not need to be extracted by solvent,could directly enter the solid phase extraction column,eluted by acetonitrile,and concentrated by nitrogen blowing and fixed volume,then detected by liquid chromatography-mass spectrometry,and quantified by internal standard method.The effects of the type of column packing,the amount of packing,elution solvent and elution volume on the extraction efficiency were investigated.Studies had shown:under optimized conditions,the linear range of benzo (a) pyrene was 0.5~10.0 ng/mL,the correlation coefficient was greater than or equal to 0.999,the detection limit was 0.1 μg/kg,and the limit of quantification was 0.4 μg/kg.The recovery rate of the samples at the three levels of 0.4 μg/kg,1.0 μg/kg and 10.0 μg/kg was 77.5%~94.8%,and the relative standard deviation was 0.65%~4.72%.The method is simple,fast,and highly accurate.The detection limit can meet the detection requirements of benzo (a) pyrene residues in edible oils and fats,and the analysis cost is low.It can provide a reference for the determination of benzo (a) pyrene in other products.

关 键 词：固相萃取技术 液相色谱-串联质谱法 苯并(A)芘 大气压化学电离 

分 类 号：TS207.5[轻工技术与工程—食品科学] O657.63[轻工技术与工程—食品科学与工程]