食品科学 ›› 2009, Vol. 30 ›› Issue (6): 163-166.doi: 10.7506/spkx1002-6630-200906035

• 分析检测 • 上一篇    下一篇

高效液相色谱法测定食品中的二苯胺残留量

罗晓燕   

  1. 广州市疾病预防控制中心
  • 收稿日期:2008-04-01 修回日期:2008-06-20 出版日期:2009-03-15 发布日期:2010-12-29
  • 通讯作者: 罗晓燕 E-mail:gzcdclxy@hotmail.com
  • 基金资助:

    卫生部2006 年食品标准制修订计划项目(41)

Determination of Diphenylamine Residue in Food by HPLC

LUO Xiao-yan   

  1. (Guangzhou Centre for Disease Control and Prevention, Guangzhou 510080, China)
  • Received:2008-04-01 Revised:2008-06-20 Online:2009-03-15 Published:2010-12-29
  • Contact: LUO Xiao-yan E-mail:gzcdclxy@hotmail.com

摘要:

目的:建立固相萃取柱净化高效液相色谱法测定食品中二苯胺残留量的方法。方法:样品经固相萃取柱净化后进行高效液相色谱测定。色谱柱为AQ-C18(250mm × 4.6mm,5 μ m),流动相为甲醇-0.02mol/L NH4Ac(pH4.2,72:28,V/V),流速为1.0ml/min,二极管阵列检测器,检测波长为285nm。结果:该方法的线性范围为:0.050~10.0 μ g/ml;标准曲线线性良好,其回归方程及相关系数为y=136.39x - 0.13,r = 0.9999。检出限为0.10mg/kg,回收率在88.0%~100% 之间,相对标准偏差小于7.0%。结论:该方法操作简便、快捷,是食品中二苯胺残留量快速而准确的检测方法。

关键词: 二苯胺, 固相萃取, 液相色谱法, 食品, 残留分析

Abstract:

Objective: An analytic method with SPE-HPLC was developed to determine diphenylamine residue in food. Method: Food was extracted with CH3OH and purified by SPE,then determined by HPLC. The chromatographic column was AQ-C18 (250 mm×4.6 mm, 5 μm), the mobile phase was methanol-0.02 mol/L NH4Ac (72:28, V/V) with the flow rate of 1.0 ml/min, and the DAD detection wavelength was 285 nm. Results: The linear range of this method is 0.050 to 10.0 μg/ml. The standard curve is well linear, and the regression equation is y=136.39x-0.13, r = 0.9999. The limit of detection is 0.10 mg/kg, the recovery is 88.0% to 100% and the relative standard deviation is less than 7.0%. Conclusion: The method is satisfying in precision, accuracy and sensitivity of determining residue of diphenylamine in food.

Key words: diphenylamine, SPE, HPLC, food, residue analysis

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