固相萃取-液相色谱法测定蜜饯中7种常见合成色素
目的 建立一种同时测定蜜饯中7种常见合成色素(柠檬黄、苋菜红、胭脂红、日落黄、亮蓝、诱惑红、赤藓红)的固相萃取-高效液相色谱(solid-phase extraction-high performance liquid chromatography, SPE-HPLC)分析方法。 方法 样品经水提取后, 采用Anpelclean PA聚酰胺SPE小柱净化, 氮吹后定容, 以甲醇和20 mmol/L乙酸铵为流动相, 通过Waters 公司XBridge C18柱梯度洗脱分离, 在特异性波长下进行测定。结果 7种常见合成色素在0.50~10.0 μg/mL范围内峰面积与其实际浓度线性相关性良好(r2≥0.9987), 在0.5、2.5、5.0 mg/kg三个加标水平上回收率在74.3%~97.5%之间, RSD在0.47%~4.80%之间。检出限在0.02~0.10 mg/kg之间, 定量限在0.06~0.30 mg/kg之间。结论 本方法灵敏度高, 分离效果好, 精密度好, 准确度高, 适用于蜜饯中7种常见合成色素的测定。
Objective To establish a method for simultaneous determination of 7 kinds of synthetic pigments (lemon yellow, amaranth, ponceau 4r, sunset yellow, coomassie brilliant blue, allura red and erythrosine) in preserved fruits with solid-phase extraction-high performance liquid chromatography (SPE-HPLC). Methods The homogenized samples were extracted by water, purified by Anpelclean PA- SPE column, and adjusted to constant volume after nitrogen blowing. HPLC analysis was conducted using methanol and 20 mmol/L ammonium acetate as mobile phase with a xbridge-C18 column from Waters company for gradient elution and separation. Specific wavelengths were applied for quantitative detection of the synthetic pigments in the samples. Results There was a good linearity between peak areas and concentrations of 7 kinds of synthetic pigments in the concentration range of 0.50~10.0 μg/mL (r2≥0.9987). The recovery rates fell in the scope of 74.3%~97.5% and RSDs ranged from 0.47% to 4.80% under the standard addition levels of 0.5, 2.5 and 5.0 mg/kg. The detection limits were between 0.02 and 0.10 mg/kg and the quantification limits between 0.06 and 0. 30 mg/kg. Conclusion The method has high sensitivity, good separation effect, good precision and high accuracy, thus, it’s suitable for the simultaneous determination of 7 kinds of common fruit pigments in preserved fruits.
标题：固相萃取-液相色谱法测定蜜饯中7种常见合成色素
英文标题：Determination of 7 kinds of synthetic pigments in preserved fruits by solid-phase extraction-high performance liquid chromatography
作者：
黄志强 建德市疾病预防控制中心
王飞 建德市疾病预防控制中心
俞文妍 建德市疾病预防控制中心
杨献青 建德市疾病预防控制中心
中文关键词:固相萃取,蜜饯,合成色素,高效液相色谱法,
英文关键词:solid-phase extraction,preserved fruits,synthetic pigments,high performance liquid chromatography,
发表日期：2015-04-27
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