摘要
合成色素由于其芳香结构的特殊性,具有高毒性和高残留,因此食用染色大米会对人体健康产生极大的危害。该文建立高效液相色谱-飞行时间质谱定性检测大米中52种限用合成色素的方法。样品经过正己烷、水和乙腈、1%氨水-甲醇分3级提取。采用XDB-C18液相色谱柱分析,正离子模式采用1%甲酸水溶液和乙腈为流动相梯度洗脱,负离子模式采用20 mmol/L乙酸铵水溶液和乙腈作为流动相梯度洗脱,ESI全扫描模式检测。结果表明：52种合成色素分别得到有效提取,加标回收率为80%-102%。通过优化锥孔电压,得到52种合成色素的最大丰度分子离子峰,与标准物质谱图数据库的匹配度均达到95%以上。该定性检测方法对大米中滥用色素筛查具有良好的适应性。
Synthetic pigment in dyed rice is harm to human health because of its special aromatic structure as well as high toxicity and high residual. HPLC-TOF/MS is introduced in this paper to determine 52 kinds of limitative synthetic pigment in rice. First, samples are extracted with n-hexane, acetonitrile and water, and 1% aqueous ammonia-methanol in succession; second, a XDB-C18 HPLC column is used for analysis; third,1% aqueous formic acid and acetonitrile are used for mobile phase gradient elution in positive ion mode while 20 mmol/L ammonium acetate and acetonitrile are used for mobile phase gradient elution in negative ion mode; and the last step is ESI full scan testing. The results show that all the synthetic pigment is efficiently extracted,with an adding standard recovery of 80% to 102%. Cone voltage is optimized to acquire the most abundant molecular ion peaks of the synthetic pigment, matching with the results in reference material spectra databases by more than 95%. This qualitative detection method has good adaptability in screening the rice with synthetic pigment.
出处
《中国测试》
CAS
北大核心
2016年第3期48-52,共5页
China Measurement & Test
基金
四川省科技厅科技支撑计划项目(2013NZ0040)
