建立了固相萃取-液相色谱/串联质谱(solid phase extraction-liquid chromatography-tandem mass spectrometry,SPE-LC/MS)同时分析静宁烧鸡中14种杂环胺(heterocyclic amines,HAAs)含量的方法。试验首先优化了14 种HAAs的仪器参数,待测样品以乙酸乙酯和NaOH提取,经PRS和C18固相萃取小柱串联净化,V(甲醇)∶V(氨水)=19∶1洗脱,将洗脱液混匀过有机滤膜上机检测。结果表明,14种HAAs在1~500 μg/L线性良好,相关系数均不低于0.999,检出限(S/N=3)为0.06~0.17 μg/kg,定量限(S/N=10)为0.19~0.58 μg/kg。14种HAAs在加标水平为20、50、100 μg/L时的回收率分别为85.75%~99.14%、85.95%~101.17%、83.04%~103.78% 。结果显示该方法线性范围宽、精密度和准确度较高、分析时间短、净化效果好、可满足肉制品中多种HAAs含量同时检测的要求。
A solid phase extraction-liquid chromatography-tandem mass spectrometry (SPE-LC/MS) method was established to sim- ultaneously analyze the contents of 14 heterocyclic amines (HAAs) in Jingning traditional braised chicken. This study firstly optimized the instrument parameters of 14 HAAs, and the meat samples were extracted with ethyl acetate and NaOH, purified by PRS and C18 cartridges in series, and eluted with methanol-ammonia (19∶1, V/V).The eluate was mixed and tested on an organic filter.The results showed that the 14 HAAs had good linearity in the concentration range of 1-500 μg/L, the correlation coefficient was not less than 0.999, the detection limit(S/N=3)was 0.06-0.17 μg/kg, the limit of quantification (S/N=10) was 0.19-0.58 μg/kg.The recoveries of 14 HAAs at spiked levels of 20, 50, and 100 μg/L were 85.75%-99.14%, 85.95%-101.17%, 83.04%-103.78%, respectively.The results showed that the method had a wide linear range, high precision and accuracy, short analysis time, and good purification effect, which could meet the requirements of simultaneous detection of multiple HAAs residues in meat products.
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