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標題: QuEChERS結合氣相層析質譜術於肉類樣品中乙型受體素檢測之研究
Determination of β-agonists in Meat Samples Using QuEChERS Extraction Coupled with Gas Chromatography-Mass Spectrometry
作者: 施衍任
Shih, Yen-Jen
關鍵字: QuEChERS;β-agonists;氣相層析質譜術;乙型受體素;Meat Samples;QuEChERS;Gas Chromatography-Mass Spectrometry
出版社: 化學系所
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本研究主要為開發肉類中微量乙型受體素之檢測方法。利用QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe)樣品前處理方法結合氣相層析質譜術(gas chromatography-mass spectrometry,GC-MS)中電子游離法之選擇離子模式(electron ionization-selected ions monitoring,EI-SIM)進行偵測。所檢測乙型受體素成分為 clenbuterol、salbutamol、terbutaline、ractopamine、cimaterol及tulobuterol等六種分析物。實驗結果QuEChERS最佳化條件為取2克之肉類樣品加入8毫升50%乙腈水溶液,於添加0.5克氯化鈉及1.8克之無水硫酸鎂後,震盪1分鐘後以4000 rpm轉速離心5分鐘。取出上清液3毫升添加0.5克無水硫酸鎂及40毫克石墨碳黑(graphitized carbon black,GCB)於之15毫升聚丙烯塑膠管中,震盪1分鐘後以4000 rpm轉速離心5分鐘,取上清液1.9毫升並以氮氣吹乾後,加入乙酸乙酯150 μL回溶並添加50 μL N,O-bis(trimethylsilyl)acetamide (BSA)衍生化後使用氣相層析質譜術檢測。方法確效方面,線性範圍除ractopamine之線性範圍為5 ng/g至1000 ng/g外,其餘分析物皆在0.5 ng/g至1000 ng/g,線性相關係數都在0.9950以上,方法偵測極限介於10 pg/g至 269 pg/g之間,同日內與異日間精密度之相對標準差分別介於2.3 %至14.2 %與3.6 %至19.3 %之間,而回收率介於76.6 %至117.7 %之間,並將此方法應用於真實肉類樣品上,實驗結果顯示真實樣品中並未測出含有乙型受體素。本研究方法具有簡單、快速及具靈敏度等優點,可作為肉類中乙型受體素檢測方法之參考。

In this study, a quick and sensitive analytical method was developed for determination of trace clenbuterol, salbutamol, terbutaline, cimaterol, tulbuterol and ractopamine in meat samples by using Quick, Easy, Cheap, Effective, Rugged, and Safe (QuEChERS) extraction technique combined with gas chromatography-mass spectrometry (GC-MS) with eletron ionization-selected ion monitoring (EI-SIM)mode.
2 g of meat samples was weighed and placed in a 15 mL Falcon centrifuge tube and then 8 mL 50 % acetonitrile aqueous solution were added in the same tube. After manual shaking for 1 min, 1.8 g anhydrous magnesium sulphate and 0.5 g sodium chloride were added into the tube then vortex for 1 min. After centrifuging at 4000 rpm for 5 min, an aliquot of 3 mL supernatant was transferred to another 15 mL Falcon centrifuge tube containing 40 mg graphitized carbon black (GCB) sorbent and 0.5 g anhydrous magnesium sulphate. After vortex for 1 min, the supernatant was transferred into a glass vial then dried by nitrogen stream. The extracts were derivatized by adding 150 μL ethyl acetate (EA) and 50 μL N,O-bis(trimethylsilyl)acetamide (BSA) and then 1 μL of extracts derivatized was injected into GC-MS. The linear ranges for clenbuterol, salbutamol, terbutaline, cimaterol, and tulbuterol were from 0.5 ng/g to 1000 ng/g and for ractopamine was from 5 ng/g to 1000 ng/g with coefficients of determination (R2) above 0.9950 for studied compound. The limits of detection were from 10 pg/g to 269 pg/g. Intra-day and inter-day precisions represented by relative standard deviation (RSD) were in the range of 2.3-14.2% and 3.6-19.3%, respectively. The application of method proposed to detect of β-agonists in real sample was tested by analyzing beef and pork samples from traditional market in Taichung . The results showed no β-agonists was detected in the beef and pork samples.
其他識別: U0005-0808201317092600
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