食品科学

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固相萃取-超高效液相色谱法快速检测辣椒面中刚果红

钟慈平1,魏 炜1,王正虹2,邱 宏2,胡黎黎2,顾万江2,甘 源2,唐小琴2,李 林3,*   

  1. 1.西南大学食品科学学院,重庆 400716;2.重庆市疾病预防控制中心,重庆 400042;
    3.西南大学校医院,重庆 400716
  • 出版日期:2014-05-25 发布日期:2014-05-29
  • 通讯作者: 李 林

Determination of Congo Red in Chili Powder by Solid Phase Extraction Coupled with Ultra-High Performance Liquid Chromatography

ZHONG Ci-ping1, WEI Wei1, WANG Zheng-hong2, QIU Hong2, HU Li-li2, GU Wan-jiang2, GAN Yuan2, TANG Xiao-qin2, ,*   

  1. 1. College of Food Science, Southwest University, Chongqing 400716, China; 2. Chongqing Center for Disease Control and
    Prevention, Chongqing 400042, China; 3. Hospital of Southwest University, Chongqing 400716, China
  • Online:2014-05-25 Published:2014-05-29
  • Contact: LI Lin

摘要:

目的:建立测定辣椒面中刚果红染料含量的超高效液相色谱方法。方法:采用氨水-乙醇(30∶70,V/V)提取剂,超声加热辅助提取3 次,合并提取液、浓缩后过HLB固相萃取小柱,以5 mL 1%甲酸-甲醇溶液淋洗、5 mL10%氨水-甲醇溶液洗脱,收集洗脱液、氮吹浓缩后定容测定。使用BEH C18色谱柱(50 mm×2.1 mm,1.7 μm);流动相:A为乙腈,B为10 mmol/L乙酸铵溶液,梯度洗脱;流速0.4 mL/min;检测波长498 nm;柱温40 ℃。结果:回收率为72%~96%,方法检出限为0.029 0 mg/kg,相对标准偏差为2.16%~5.97%(n=6),线性方程相关系数达到0.999 9。结论:本方法简便、快速、准确、灵敏,适用辣椒面中刚果红染料含量的测定。

关键词: 超高压液相色谱, 辣椒面, 刚果红, 含量测定

Abstract:

Objective: To establish a method for determining Congo red in chili powder by ultra-high performance liquid
chromatography (UPLC). Methods: Samples were extracted with a mixture of ammonia and ethanol (30:70, V/V). The
extraction process was aided by ultrasonic treatment and repeated three times. The combined extract was concentrated
and then clean-up on an HLB solid-phase extraction cartridge by washing with 5 mL of 1% formic acid in methanol
and elution with 5 mL of 10% ammonia in methanol. The collected eluate was concentrated under a stream of nitrogen
prior to analysis. The chromatographic separation was achieved within 4 min on a BEH C18 column (50 mm×2.1 mm,
1.7 μm) by gradient elution using acetonitrile as mobile phase A and 10 mmol/L ammonium acetate as mobile phase B at a
flow rate of 0.4 mL/min. The detection wavelength was set at 498 nm and the column temperature was maintained at 40 ℃.
Results: Average recoveries of Congo red from chili samples spiked three concentration levels ranged from 72% to 96% with
relative standard deviation of 2.16%–5.97% (n = 6). The detection limit of the proposed method was 0.029 0 mg/kg, and the
correlation coefficient for the calibration curve was 0.999 9. Conclusion: This method is simple, rapid, accurate, sensitive
and suitable for detecting Congo red dye in chili powder.

Key words: ultra-high performance liquid chromatography (UPLC), chili powder, Congo red, quantitative determination

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