青石斑鱼中丁香酚的残留消除特征研究

发布时间：2018-03-07 00:13

  本文选题：丁香酚　切入点：气相色谱-串联质谱法　出处：《浙江海洋大学》2017年硕士论文　论文类型：学位论文

【摘要】：首先,本文建立了三重四级杆串联质谱法测定鱼肉中的丁香酚及其异构体残留量的方法。样品使用正己烷进行提取,提取液经苯基SPE柱净化处理后使用气相色谱-串联质谱仪(GC-MS/MS)进行检测,内标法定量。色谱柱采用Agilent JW Scientific DB-17ms,以1 ml/min的氦气作载气,使用电子轰击式离子(EI)源,取m/z 149作为定量离子对目标物进行定量,并以离子m/z 104和m/z 77辅助定性。本方法在水产品中丁香酚、异丁香酚、甲基丁香酚的最低检测限分别为0.4μg/kg、1.2μg/kg、0.2μg/kg,最低定量限分别为1.2μg/kg、4μg/kg、0.7μg/kg,在空白样品中加标回收率范围在98.6%~104%。相对标准偏差范围为2.46%~5.48%。样品前处理简便,回收率较好,适用于试验中鱼肉丁香酚及其异构体残留的检测。其次,研究温控无药物辅助下石斑鱼的存活率,结果表明20℃温控无药物条件下存活率不高而且鱼活力差,无法恢复到正常状态。在25℃下用丁香酚进行辅助麻醉,70 mg/L高浓度下能够在2.1min内使鱼进入麻醉4期,并能够在4.8min内复苏,该浓度适合在实际运输中进行装车和卸货过程中进行人工操作。8 mg/L低浓度10h麻醉,结果显示,存活率能够达到100%,且最终麻醉状态为麻醉2期,(鱼体失去触觉但仍保持平衡),适合于短途运输过程中作镇静使用。最后,根据两种不同给药方式进行麻醉试验的结果,确定给药浓度进行两种不同给药方式的残留消除试验。石斑鱼鱼肉中经高浓度短时麻醉,24h后残留首次(0.148±0.907mg/kg)给药和二次(0.114±0.0562 mg/kg)给药,低浓度长时麻醉后鱼肉中富集的最高浓度达到62.3±23.1mg/kg,在清水中复苏24h后残留量为39.2±19.0mg/kg,当净化时间达到48h含量低于0.1mg/kg,达到动态平衡。人体健康风险评估显示,高浓度重复麻醉和低浓度长时麻醉的药峰浓度62.3 mg/L远低于JECFA推荐的丁香酚可接受日摄入量,水产品中丁香酚的残留对人体健康危害风险低。根据运输模拟及残留消除试验,结果表明,高浓度重复石斑鱼,鱼体能够快速麻醉,长时间麻醉后存活率高,且消除代谢快,经一定时间的贮养后能够安全食用,更适合于实际生产过程中使用。因此,为丁香酚列入我国合法鱼用麻醉剂的候选名单提供参考。
[Abstract]:Firstly, a method for the determination of eugenol and its isomer residues in fish by triple four-step tandem mass spectrometry was established. The samples were extracted by n-hexane. The extracted solution was purified by phenyl SPE column and detected by GC-MS / MS with gas chromatography-tandem mass spectrometer (GC-MS / MS). The chromatographic column was Agilent JW Scientific DB-17ms. using 1 ml/min helium as carrier gas and electron bombardment ion (EI) source. Using m / z 149 as the quantitative ion to quantify the target material, and with the aid of ion m / z 104 and m / z 77, the method is used to determine eugenol, isoeugenol, eugenol and eugenol in aquatic products. The minimum detection limit of methyleugenol is 0.4 渭 g / kg ~ (-1) 渭 g / kg ~ (-1) 渭 g / kg ~ (0.2) 渭 g 路kg ~ (-1), and the lowest quantitative limit is 1.2 渭 g / kg ~ (4) 渭 g / kg ~ (-1) 渭 g / kg ~ (0.7) 渭 g 路kg ~ (-1) 路kg ~ (-1), respectively. The recoveries are in the range of 98.6 渭 g / kg ~ (104). The relative standard deviation range is 2.465.48. The sample pretreatment is simple and the recovery is good. It is suitable for the detection of eugenol and its isomer residues in fish meat. Secondly, the survival rate of grouper was studied under the condition of temperature control without drugs. The results showed that the survival rate of grouper was not high and the activity of fish was poor under the condition of 20 鈩，

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