(重庆市计量质量检测研究院/重庆市食品安全工程技术研究中心/国家农副加工产品及调味品 质量监督检验中心, 重庆 401123)
(Chongqing Academy of Metrology and Quality Inspection/Chongqing Engineering Research Center for Food Safety/ National Center of Quality Supervision and Inspection Agricultural Processed Products and Condiments, Chongqing 401123, China)
建立了分散固相萃取-超低温液液微萃取-气相色谱质谱法测定烟熏及烧烤肉制品中16种欧盟优控多环芳烃的分析方法。样品用乙腈提取、上清液经分散固相萃取净化后在-80℃条件下采用甲苯液液微萃取浓缩,选用DB-EUPAH色谱柱(20m×0.18mm×0.14μm)分离,最后经质谱检测定量。结果表明,16种欧盟多环芳烃在5~500μg/L浓度范围内线性关系良好,相关系数均大于0.999,对烟熏和烧烤的肉制品进行3个不同浓度的加标实验,平均回收率为75.2%~114.2%,RSD为1.84%~7.57% (n=6),检出限(S/N=3)为0.1~0.5μg/kg。 应用该方法对40批次市售腊肉制品和烤肉制品中多环芳烃进行了检测,发现部分腊肉制品和烤肉制品中多环芳烃含量超过相关标准和法规的限量要求。 该检测方法成本低,灵敏可靠,同时符合国家标准和欧盟法规对烟熏及烧烤肉制品中多环芳烃的限量检测要求。
A fast and low-cost determination method of 16 EU (European Union) priority polycyclic aromatic hydrocarbons (PAHs) in smoked and roasted meat products by dispersive solid-phase extraction with ultra-low temperature liquid-liquid microextraction combined with gas chromatography-mass spectrometry (GC-MS) analysis was developed. The samples were extracted by acetonitrile, and the supernatants were purified using mixed adsorbent by dispersive solid-phase extraction and then extracted by methylbenzene using liquid-liquid microextraction at -80℃. The analytes were separated on a DB-EUPAH high resolution gas chromatography column (20m×0.18mm×0.14μm), and the data were collected by single ion monitoring mass spectrometry, followed by qualitative screening and quantitative analysis. The result showed that the linear relationship of 16 EU priority PAHs at the concentration range of 5-500μg/L were good, and the correlation coefficients were greater than 0.999. Smoked and roasted meat products were spiked at three levels, the average recoveries of 16 EU priority PAHs ranged from 75.2%-114.2% with RSDs of 1.84%-7.57% (n=6). The limits of detection (S/N=3) were 0.1-0.5μg/kg. This method was applied to detect PAHs in 40 batches of smoked and roasted meat on market, and it was found that the content of PAHs in some smoked and roasted meat exceeded the requirements of relevant standards and regulations. The detection method had the advantages including low cost, sensitive, and reliable, which also met the requirements of national standard and EU regulation for the limited detection of PAHs in smoked and roasted meat.