CAJ | 학술논문

建立了河豚鱼、鳗鱼和烤鳗中角黄素残留的超高效液相色谱测定方法和超高效液相色谱-串联质谱确证方法. 样品用抗氧化剂焦性没食子酸保护, 乙腈均质提取, 正己烷液-液分配净化, 超高效液相色谱-紫外检测器测定, 外标法定量, 超高效液相色谱-串联质谱法确证. 测定方法采用BEHC18色谱柱(50 mm×2.1 mm, i.d. 1.7 μm), 流动相为V(0.1%的甲酸)∶V(乙腈)＝3∶97, 检测波长470 nm. 实验结果表明, 角黄素在0.05～2.0 mg/L范围内线性关系良好(r=0.9999), 在空白样品中, 添加低、中、高3个浓度水平(0.05, 0.1, 1.0 mg/kg), 角黄素的回收率均在82.52%～96.96%之间, 相对标准偏差为6.9%～15%. 方法的检出限(LOD)为 0.02 mg/kg, 定量限(LOQ) 为0.05 mg/kg. 串联质谱确证方法采用电喷雾(ESI)离子源, 在正离子模式下以多反应监测(MRM)扫描方式检测, 定性离子对565.5/203.2和565.5/133.1, 定量离子对565.5/203.2.
건립료하돈어、만어화고만중각황소잔류적초고효액상색보측정방법화초고효액상색보-천련질보학증방법. 양품용항양화제초성몰식자산보호, 을정균질제취, 정기완액-액분배정화, 초고효액상색보-자외검측기측정, 외표법정량, 초고효액상색보-천련질보법학증. 측정방법채용BEHC18색보주(50 mm×2.1 mm, i.d. 1.7 μm), 류동상위V(0.1%적갑산)∶V(을정)＝3∶97, 검측파장470 nm. 실험결과표명, 각황소재0.05～2.0 mg/L범위내선성관계량호(r=0.9999), 재공백양품중, 첨가저、중、고3개농도수평(0.05, 0.1, 1.0 mg/kg), 각황소적회수솔균재82.52%～96.96%지간, 상대표준편차위6.9%～15%. 방법적검출한(LOD)위 0.02 mg/kg, 정량한(LOQ) 위0.05 mg/kg. 천련질보학증방법채용전분무(ESI)리자원, 재정리자모식하이다반응감측(MRM)소묘방식검측, 정성리자대565.5/203.2화565.5/133.1, 정량리자대565.5/203.2.
A method was developed for the determination of canthaxanthin residues in fugu, eel and roast eel by ultra performance liquid chromatography equipped with an UV detector (UPLC-UV) and confirmation by ultra performance liquid chromatography equipped with tandem mass spectrometry (UPLC-MS/MS) . Under the protection of antioxidant pyrogallic acid, the samples were extracted with acetonitrile by homogenizer, and cleaned up by liquid-liquid extraction with n-hexane, then determined by UPLC-UV and confirmed by UPLC-MS/MS, quantified by the external standard method. For determination, BEHC18 column (50 mm×2.1 mm, i.d., 1.7 μm) was used, mobile phase was 0.1% formic acid-acetonitrile (3:97, vlv), at a flow rate of 0.4 mL/rnin, detection wavelength was 470 run. Trie calibration curve was linear between the area and the concentration of canthaxanthin from 0.05 to 2.0 mg/L, the correlation coefficient was 0.9999. The average recoveries for the spiked fugu, eel and coast eel at the concentrations of 0.05, 0.1, 1.0 mg/kg ranged from 82.52% to 96.%% with relative standard deviation less than 14.8%. The limit of detection (LOD) was 0.02 mg/kg and the limit of quantity (LOQ) was 0.05 mg/kg. For confirmation, electrospray ionization was applied and operated in the positive ion with multiple reaction monitoring (MRM) scan mode in MS/MS analysis.