超声提取-气相色谱-串联质谱法测定煎烤鱿鱼中16种多环芳烃

本实验建立了超声提取-气相色谱-串联质谱法（polycyclic aromatic hydrocarbons, PAHs）测定煎烤鱿鱼中16种多环芳烃的分析方法。考察了提取试剂配比、提取试剂用量、提取温度等对回收率的影响，确定了最佳的提取和检测方法:5.00 g样品冷冻干燥后经25 mL正己烷30 ℃超声提取20 min，复提一次，经碱性氧化铝-中性硅胶复合固相萃取柱净化后，采用气相色谱-串联质谱法测定，多环芳烃氘代内标法定量。在此实验条件下，16种目标物在1~100 ng/mL范围内呈良好线性关系，线性相关系数（r）不低于0.9994，检出限为0.09~0.52 μg/kg，定量限为0.21~1.21 μg/kg。在1、2、20 μg/kg 3个加标水平下回收率分别为73.98%~128.17%、73.21%~133.24%、76.35%~133.68%，相对标准偏差（RSD，n=6）分别为1.32%~2.98%、0.93%~2.47%、1.08%~2.87%。在实际样品检测应用中，6个样品均有不同程度的多环芳烃检出，单一组分检出范围从0~48.65 μg/kg不等。结果表明，该方法选择性好，可用于煎烤鱿鱼中多环芳烃的检测，也可应用于其他类似的加工水产品中多环芳烃的提取与检测。

Determination of 16 Polycyclic Aromatic Hydrocarbons(PAHs) in Fried Squid by Ultrasonic Extraction-Gas Chromatography-Mass Spectrometry

In this experiment, an analytical method for the determination of 16 PAHs in fried squid by ultrasonic extraction-gas chromatography-mass spectrometry (PAHs) was established. The effects of extraction reagent ratio, extraction reagent dosage and extraction temperature on the recovery rate were investigated. The best extraction and detection method was determined as follows: after freeze-drying, 5.00 g sample was extracted by 25 mL n-hexane at 30 ℃ for 20 min, and then reextracted once. After purification by alkaline alumina neutral silica gel composite solid phase extraction column, compounds was determined by gas chromatography tandem mass spectrometry and quantified by deuterium internal standard method. Under these experimental conditions, 16 target compounds showed good linear relationship in the range of 1~100 ng/mL, the linear correlation coefficient (r) was not less than 0.9994, the detection limit was 0.09~0.52 μg/kg, and the quantitation limit was 0.21~1.21 μg/kg. The recoveries were 73.98%~128.17%, 73.21%~133.24% and 76.35%~133.68% at the spiked levels of 1, 2 and 20 μg/kg, respectively. The relative standard deviations (RSD, n=6) were 1.32%~2.98%, 0.93%~2.47% and 1.08%~2.87%, respectively. In the actual sample detection application, PAHs were detected in all the six samples. The detection range of single component ranged from 0 to 48.65 μg/kg. The results showed that the method had good selectivity. It could be used for the detection of polycyclic aromatic hydrocarbons in fried squid and other similar processed aquatic products.