超高效液相色谱-四极杆串联离子阱复合质谱法测定肉制品中非法添加的碱性工业染料

Determination of illegally added basic industrial dyes in meat products by ultra performance liquid chromatography-quadrupole tandem ion trap combined mass spectrometry

中文关键词:  肉制品  碱性工业染料  超高效液相色谱-四极杆串联离子阱复合质谱法

英文关键词:meat products  basic industrial dyes  ultra performance liquid chromatography-quadrupole tandem ion trap combined mass spectrometry

中文摘要:

      目的 建立超高效液相色谱-四极杆串联离子阱复合质谱法检测肉制品中7种工业染料的方法。方法 样品经醋酸乙腈提取, WCX固相萃取柱净化, C18色谱柱分离, 以甲醇和0.1%甲酸水溶液为流动相进行梯度洗脱, 电喷雾正离子模式电离, 多反应监测(multiple response monitoring, MRM)→信息相关采集(information dependent acquisition, IDA)→增强子离子扫描(enhanced product ion, EPI)模式检测, 外标法定量。结果 7种碱性工业染料在0.01~2.00 μg/mL范围内均呈现良好的线性关系, 相关系数(r)均大于0.995。检出限为0.4~3.6 μg/kg, 平均加标回收率为68.9%~99.9%, 相对标准偏差为4.8%~8.4%。结论 本方法应用超高效液相色谱-四极杆串联离子阱复合质谱特有的MRM-IDA-EPI扫描模式, 可同时实现化合物的准确定性、定量分析及可疑峰筛查、确证。

英文摘要:

      Objective To establish a method for the determination of 7 kinds of industrial dyes in meat products by ultra performance liquid chromatography-quadrupole tandem ion trap combined mass spectrometry. Methods The samples were extracted with acetonitrile acetate, purified by WCX solid-phase extraction column, and separated on a C18 chromatographic column. Gradient elution was performed using methanol and 0.1% formic acid aqueous solution as the mobile phase, followed by electrospray positive ion mode ionization, multiple response monitoring (MRM)→information dependent acquisition (IDA)→enhanced product ion (EPI) mode detection, and quantification was conducted by external standard method. Results The linear relationships of the 7 kinds of basic industrial dyes were good in the range of 0.01?2.00 μg/mL, and the correlation coefficients (r) were greater than 0.995. The limits of detection were 0.4?3.6 μg/kg, the average recoveries were 68.9%-99.9%, and the relative standard deviations were 4.8%?8.4%. Conclusion In the method, the MRM-IDA-EPI scanning mode unique to the ultra performance liquid chromatography-quadrupole tandem ion trap composite mass spectrum is applied, and accurate qualitative and quantitative analysis of the compound as well as suspicious peak screening and confirmation can be realized simultaneously.