利用超高效液相色谱-四极杆飞行时间质谱（ UPLC-Q-TOF MS）技术建立了水产品中28种酸性合成色素的快速检测方法。水产样品采用氨水-水-乙醇（2：1：7，v／v／v）溶液提取，经氨基化吸附剂基质分散法净化后直接用UPLC-Q-TOF MS测定。目标物经 Eclipse Plus-C18柱分离，以0.1％（ v／v）甲酸-5 mmol／L乙酸铵水溶液和乙腈为流动相进行梯度洗脱，采用电喷雾负离子模式下全信息串联质谱扫描模式进行检测。结果表明：水产品中28种酸性合成色素的定量限（ LOQ，S／N=10）为20~100μg／kg；并在各自的线性范围内线性关系良好（相关系数 r）≥0.991，峰面积的相对标准偏差（ n=6）均小于5.61％；在3个加标水平下的平均回收率为70.24％~106.47％，相对标准偏差为5.62％~9.65％（ n=6）。该方法快速简单、灵敏度高，适用于水产品中28种色素的快速筛查。
An analytical method was established for the simultaneous determination of 28 acidic artificial dyes in fishery products by ultra performance liquid chromatography coupled with qua-drupole-time of flight mass spectrometry( UPLC-Q-TOF MS). The analytes in fishery products were extracted with ethyl alcohol containing 20%( v/v)ammonia water and 10%( v/v)water. Then the extract solution was purified according to amination adsorbent matrix dispersion method. The compounds were separated by an Eclipse Plus-C 18 column with acetonitrile and 0. 1%(v/v)formic acid-5 mmol/L ammonium acetate solution as the mobile phases,and measured by UPLC-Q-TOF MS with electrospray ionization in negative mode. As a result,the limits of quantification( LOQs,S/N = 10 ) of the target compounds were 20-100 μg/kg in fishery products. The 28 analytes behaved linearly in wide-range with the correlation coeffi-cients more than 0. 991 as well as the relative standard deviations( RSDs)of the peak areas less than 5. 61%( n = 6 ). The average recoveries of the 28 analytes spiked at three levels were ranged from 70. 24% to 106. 47% with RSDs of 5. 62%-9. 65%( n= 6 ). This method can be applied to the analysis of the 28 acidic artificial dyes in fishery products due to its fastness ,sim-plicity and relatively high sensitivity.
参考文献
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| [2] | Feng, F.;Zhao, Y.;Yong, W.;Sun, L.;Jiang, G.;Chu, X..Highly sensitive and accurate screening of 40 dyes in soft drinks by liquid chromatography-electrospray tandem mass spectrometry[J].Journal of chromatography, B. Analytical technologies in the biomedical and life sciences,201120(20):1813-1818. |
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