本文選題：丁香酚　切入點(diǎn)：氣相色譜-串聯(lián)質(zhì)譜法　出處：《浙江海洋大學(xué)》2017年碩士論文　論文類型：學(xué)位論文

【摘要】：首先,本文建立了三重四級桿串聯(lián)質(zhì)譜法測定魚肉中的丁香酚及其異構(gòu)體殘留量的方法。樣品使用正己烷進(jìn)行提取,提取液經(jīng)苯基SPE柱凈化處理后使用氣相色譜-串聯(lián)質(zhì)譜儀(GC-MS/MS)進(jìn)行檢測,內(nèi)標(biāo)法定量。色譜柱采用Agilent JW Scientific DB-17ms,以1 ml/min的氦氣作載氣,使用電子轟擊式離子(EI)源,取m/z 149作為定量離子對目標(biāo)物進(jìn)行定量,并以離子m/z 104和m/z 77輔助定性。本方法在水產(chǎn)品中丁香酚、異丁香酚、甲基丁香酚的最低檢測限分別為0.4μg/kg、1.2μg/kg、0.2μg/kg,最低定量限分別為1.2μg/kg、4μg/kg、0.7μg/kg,在空白樣品中加標(biāo)回收率范圍在98.6%~104%。相對標(biāo)準(zhǔn)偏差范圍為2.46%~5.48%。樣品前處理簡便,回收率較好,適用于試驗中魚肉丁香酚及其異構(gòu)體殘留的檢測。其次,研究溫控?zé)o藥物輔助下石斑魚的存活率,結(jié)果表明20℃溫控?zé)o藥物條件下存活率不高而且魚活力差,無法恢復(fù)到正常狀態(tài)。在25℃下用丁香酚進(jìn)行輔助麻醉,70 mg/L高濃度下能夠在2.1min內(nèi)使魚進(jìn)入麻醉4期,并能夠在4.8min內(nèi)復(fù)蘇,該濃度適合在實際運(yùn)輸中進(jìn)行裝車和卸貨過程中進(jìn)行人工操作。8 mg/L低濃度10h麻醉,結(jié)果顯示,存活率能夠達(dá)到100%,且最終麻醉狀態(tài)為麻醉2期,(魚體失去觸覺但仍保持平衡),適合于短途運(yùn)輸過程中作鎮(zhèn)靜使用。最后,根據(jù)兩種不同給藥方式進(jìn)行麻醉試驗的結(jié)果,確定給藥濃度進(jìn)行兩種不同給藥方式的殘留消除試驗。石斑魚魚肉中經(jīng)高濃度短時麻醉,24h后殘留首次(0.148±0.907mg/kg)給藥和二次(0.114±0.0562 mg/kg)給藥,低濃度長時麻醉后魚肉中富集的最高濃度達(dá)到62.3±23.1mg/kg,在清水中復(fù)蘇24h后殘留量為39.2±19.0mg/kg,當(dāng)凈化時間達(dá)到48h含量低于0.1mg/kg,達(dá)到動態(tài)平衡。人體健康風(fēng)險評估顯示,高濃度重復(fù)麻醉和低濃度長時麻醉的藥峰濃度62.3 mg/L遠(yuǎn)低于JECFA推薦的丁香酚可接受日攝入量,水產(chǎn)品中丁香酚的殘留對人體健康危害風(fēng)險低。根據(jù)運(yùn)輸模擬及殘留消除試驗,結(jié)果表明,高濃度重復(fù)石斑魚,魚體能夠快速麻醉,長時間麻醉后存活率高,且消除代謝快,經(jīng)一定時間的貯養(yǎng)后能夠安全食用,更適合于實際生產(chǎn)過程中使用。因此,為丁香酚列入我國合法魚用麻醉劑的候選名單提供參考。
[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，

本文編號：1577106