河豚鱼、鳗鱼和烤鳗中角黄素残留的超高效液相色谱法测定和超高效液相色谱-串联质谱法确证  

Ultra performance liquid chromatographic determination and ultra performance liquid chromatography-tandem mass spectrometric confirmation of anthaxanthin residues in fugu,eel and roast eel

作　　者：薄海波 星玉秀[2] 雒丽丽[3] 贾光群[4] 庞国芳[4] 

机构地区：[1]青海出入境检验检疫局,西宁810000 [2]中国科学院西北高原生物研究所,西宁810000 [3]甘肃农业大学,兰州730070 [4]秦皇岛出入境检验检疫局,秦皇岛066002

出　　处：《分析试验室》2009年第11期48-52,共5页Chinese Journal of Analysis Laboratory

基　　金：国家标准2007年第七批制修订计划(20079498-T-469)项目资助

摘　　要：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.1.7μm）,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。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 （UPLG-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, v/v）, at a flow rate of 0.4 mL/min, detection wavelength was 470 nm. The 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 96.96% 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.

关 键 词：角黄素 河豚鱼 鳗鱼 烤鳗 超高效液相色谱 超高效液相色谱-串联质谱 

分 类 号：O657.7[理学—分析化学] O557.63[理学—化学]