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  

Simultaneous determination of four Sudan dyes in blood bysolid-phase extraction combined with ultra-fast liquid chromatography-tandem mass spectrometry

作　　者：朱浩[1] 黄坤玉[1] 付建飞[1] 胡岳[1] 黄娴妮[1] 陈晓红[2,3] 邹宝波[1] 金米聪[2,3] 

机构地区：[1]宁波大学医学院,浙江宁波315211 [2]宁波市疾病预防控制中心,浙江省微量有毒化学物健康风险评估技术研究重点实验室,浙江宁波315010 [3]宁波市疾病预防控制中心,宁波市毒物研究与控制重点实验室,浙江宁波315010

出　　处：《色谱》2014年第3期224-229,共6页Chinese Journal of Chromatography

基　　金：浙江省自然科学基金项目(LY13B050003);浙江省分析测试项目(2013C37089);浙江省医药卫生科研项目(2013KYA187);宁波市自然科学基金项目(2013A610243)

摘　　要：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＆#215;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＆amp;nbsp;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.

关 键 词：超快速液相色谱-串联质谱法 固相萃取 苏丹染料 血液 ultra-fast liquid chromatography-tandem mass spectrometry(UFLC-MS MS) sol-id-phase extraction(SPE) 

分 类 号：O658[理学—分析化学]