气相色谱-同位素稀释质谱法测定肉中多环芳烃含量

Determination of 16 Polycyclic Aromatic Hydrocarbons in Meat Samples by Gas Chromatography-Isotope Dilution Mass Spectrometry Approach

采用分子印迹固相萃取技术,建立肉中多环芳烃残留的气相色谱-同位素稀释质谱检测方法。以萘-D8为内标、正己烷-二氯甲烷(7∶3,V/V)混合溶液为提取试剂,经过匀浆、超声提取、离心、分子印迹固相萃取等步骤,在优化仪器条件下进行定性、定量分析。在5~100 ng/mL范围内,16种多环芳烃峰面积与内标物峰面积的比值均与质量浓度的比值呈良好的线性关系,线性相关系数不小于0.999 9,肉及肉制品中检出限为0.125~0.625μg/kg。3个加标水平下的样品回收率在85.7%~109%之间,相对标准偏差(n=6)在0.75%~4.90%之间。该方法前处理效率高,定量法灵敏、准确,适合于监控肉类中多环芳烃的含量。

Using molecularly imprinted solid phase extraction, a gas chromatography-isotope dilution mass spectrometry (GC-IDMS) method was developed for the determination of polycyclic aromatic hydrocarbons (PAHs) in meat samples. Naphthalene-D8 was used as an internal standard, and a mixed solvent of n-hexane-dichloromethane (7:3, V/V) was used as an extraction solvent. The sample preparation consisted of homogenization, ultrasonic extraction, centrifugation, and purification by molecularly imprinted solid phase extraction cartridge. The qualitative and quantitative analysis were conducted under optimized instrumental conditions. The calibration curves showed a good linearity within the concentration range of 5–100 ng/mL with correlation coefficient no less than 0.999 9 and the limit of detection (LOD) was 0.125–0.625 μg/kg for meat and meat products. The recoveries at three spiked levels ranged from 85.7% to 109% with relative standard deviations (RSDs) of 0.75%–4.90%. The results indicated that this method was efficient, sensitive and accurate and could be successfully applied in the quantification of PAHs in meat.