固相萃取-超快速液相色谱-串联质谱法同时测定血液中的4种苏丹染料

摘要

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.%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。