建立了血液样品中4种苏丹染料（苏丹Ⅰ、Ⅱ、Ⅲ和Ⅳ）的固相萃取-超快速液相色谱-串联质谱（ UFLC-MS /MS）测定方法。样品经乙腈涡旋振荡提取，上清液加等体积水稀释混匀后移入 C18固相萃取小柱净化，采用 Agi-lent Eclipse Plus C18色谱柱（100 mm×2.1 mm，1.8μm）以0.1％（v / v）甲酸水溶液和0.1％（v / v）甲酸乙腈溶液为流动相梯度洗脱分离，电喷雾电离（ESI）正离子多反应监测模式进行定量分析。讨论了苏丹Ⅲ和苏丹Ⅳ的偶氮基团 E-Z 光学异构现象，并对影响因素进行了分析。结果4种苏丹染料在0.1~20.0μg / L 范围内线性关系良好，相关系数均大于0.999；在低、中、高3个加标水平的平均回收率为93.0％~108.2％，相对标准偏差为4.8％~9.5％；方法的检出限（LOD）为0.06μg / L，定量限（LOQ）为0.2μg / L。本方法准确、快速、灵敏，可用于血液样品中苏丹类染料的检测分析。
A method for the simultaneous determination of Sudan Ⅰ,Ⅱ,Ⅲ,and Ⅳ in blood samples by solid-phase extraction ( SPE ) combined with ultra-fast liquid chromatography-tandem mass spectrometry(UFLC-MS / MS)has been established. The samples were extracted with acetonitrile by vortex and vibrate technique,and then the supernatant was diluted with equal volume of water and cleaned up by a C18 SPE column. The separation was performed on an Agilent Eclipse Plus C18 column(100 mm×2. 1 mm,1. 8 μm)by gradient elution with aceto-nitrile containing 0. 1%(v / v)formic acid and 0. 1%(v / v)formic acid aqueous solution as the mobile phases. The electrospray ionization(ESI)source in the positive mode and multiple reac-tion monitoring(MRM)mode were used for the quantitative analysis. In addition,the phenom-enon of E-Z optical isomer occurred by the azo group from Sudan Ⅲ and Ⅳ was found,and the influencing factors were discussed. The results showed that the calibration curves were in good linearity for the four Sudan dyes ranged from 0. 1 to 20. 0 μg / L with the correlation coefficients of more than 0. 999. The average recoveries were from 93. 0% to 108. 2% with the relative stand-ard deviations( RSDs)from 4. 8% to 9. 5% . The limits of detection( LODs)and the limits of quantification( LOQs)were 0. 06 μg / L and 0. 2 μg / L for the four analytes,respectively. The developed method is simple,rapid,and highly sensitive. It can be used for the determination of trace Sudan dyes in blood samples.
参考文献
| [1] | Rebane R;LeitoI;YurchenkoS.[J].Journal of Chromatography A,20101217(17):2747. |
| [2] | Stiborová M;MartínekV;Ry′dlová H.[J].Cancer Research,200262(20):5678. |
| [3] | European Food Safety Authority.[J].EFSAJ,2005263:1. |
| [4] | Ahlstrom L H;EskilssonC S;BjorklundE.[J].TrendsAnal Chem,200524(01):49. |
| [5] | Valencia M C;UrozF;TafersitiY.[J].QuimAnal,200019(03):129. |
| [6] | 庞艳玲;王怀友.[J].分析试验室,200826(01):60. |
| [7] | Mo Z R;ZhangY F;ZhaoF Q.[J].FoodChem,2010121(01):233. |
| [8] | Qi Y H;ShanW C;LiuY Z.[J].Journal of Agricultural and Food Chemistry,201260(09):2116. |
| [9] | M?lder K;KünnapasA;HerodesK.[J].Journal of Chromatography A,20071160(1/2):227. |
| [10] | Zacharis C K;KikaF S;TzanavarasP D.[J].TALANTA,201184(02):480. |
| [11] | Noguerol-Cal R;López-VilariňoJ M;Fernández-MartínezG.[J].Journal of Chromatography A,20081179(02):152. |
| [12] | 刘珺;弓振斌.[J].色谱,201230(06):624. |
| [13] | He L M;SuY J;FangB H.[J].Analytica Chimica Acta,2007594(01):139. |
| [14] | 何荣;廖林川;颜有仪.[J].分析测试学报,200827(07):751. |
| [15] | Erdemir U S;IzgiB;GucerS.[J].AnalMethods,20135(07):1790. |
| [16] | 黄晓兰;吴惠勤;黄芳.[J].分析测试学报,200524(03):1. |
| [17] | Schummer C;SasselJ;BonenbergerP.[J].Journal of Agricultural and Food Chemistry,201361(09):2284. |
| [18] | Murty M R V S;SridharaC N;PrabhakarS.[J].FoodChem,2009115(04):1556. |
| [19] | Gao H;YangM L;WangM L.[J].Journal of AOAC International,201396(01):110. |
| [20] | Li C;WuY L;ShenJ Z.[J].FoodAddit Contam A,201027(09):1215. |
| [21] | 王鹏;郭少飞;荆涛.[J].色谱,200826(03):353. |
| [22] | Mejia E;DingY;MoraM F.[J].FoodChem,2007102(04):1027. |
| [23] | Polson C;SarkarP;IncledonB.[J].Journal of Chromatography B,2003785(02):263. |
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