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机构地区:[1]湖北省嘉鱼县血防医院,嘉鱼437200 [2]湖北省疾病预防控制中心,武汉430079
出 处:《食品安全质量检测学报》2014年第2期492-496,共5页Journal of Food Safety and Quality
基 金:国家自然科学基金项目(20907048);卫生公益性科研专项(200902009);中国博士后科学基金项目(20090450459);湖北省卫生厅青年人才项目(QJX2010-33)~~
摘 要:目的:建立辣椒粉中的碱性橙和碱性玫瑰精的高效液相色谱-串联四极杆质谱测定方法。方法样品经乙腈超声提取后,经 ODS-C18和乙二胺-N-丙基硅烷(PSA)的固相分散净化后直接进样分析。使用安捷伦Zobax Eclipse Plus-C18(2.1 mm×100 mm,1.8μm)色谱柱分离,以5 mmol/L乙酸铵-0.1%甲酸-乙腈为流动相,流速为0.25 mL/min。采用电喷雾离子化源,以多反应监测(MRM)方式分析,正离子化进行检测。结果碱性橙和碱性玫瑰精的线性范围为5~1000μg/L,相关系数良好。辣椒粉中碱性橙和碱性玫瑰精的检出限分别为2μg/kg和0.5μg/kg,该方法在三个水平上添加回收率为88.1%~106.4%,相对标准偏差为5.3%~11.7%。结论本方法灵敏度高,操作简单高效,适合于辣椒粉中碱性橙和碱性玫瑰精的定量及确证分析。Objective To develop a liquid chromatography-tandem mass spectrometry with solid phase dispersion for the determination of chrysoidine G and rhodamine B in paprika. Methods The sample was ul-trasonically extracted from homogenized samples with acetonitrile, and cleaned up by dispersive ODS-C18 and PSA, then determined by electrospray ionization in positive mode using multiple reactions monitoring (MRM) finally. Results There was a good linear relationship in range of 5~1000 μg/L of chrysoidine G and rhoda-mine B. The limit of detection for chrysoidine G and rhodamine B was 2μg/kg and 0.5μg/kg. The recoveries were 88.1%~106.4% of three spiked levels, and RSDs were between 5.3%~11.7% (n=6). Conclusion This method is simple, effective and sensitive, and it is suitable for the determination and confirmation of chrysoi-dine G and rhodamine B in paprika.
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