色谱

色谱

• 样品预处理方法专栏 • 上一篇    下一篇

腐殖酸键合硅胶固相萃取-液相色谱法测定辣椒粉及辣椒油中的苏丹红

郑明明,吴剑虹,骆丹,余琼卫,冯钰锜   

  1. College of Chemistry and Molecular Sciences, Wuhan University, Wuhan

    430072, China

  • 收稿日期:2007-08-14 修回日期:1900-01-01 出版日期:2007-09-30 发布日期:1985-03-25
  • 通讯作者: 冯钰锜

Determination of Sudan Red Dyes in Hot Chili Products by Humic

Acid-Bonded Silica Solid-Phase Extraction Coupled with High Performance

Liquid Chromatography

ZHENG Mingming, WU Jianhong, LUO Dan, YU Qiongwei, FENG Yuqi   

  1. College of Chemistry and Molecular Sciences, Wuhan University, Wuhan

    430072, China

  • Received:2007-08-14 Revised:1900-01-01 Online:2007-09-30 Published:1985-03-25

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摘要：

以腐殖酸键合硅胶作为固相萃取介质,建立了固相萃取柱净化、高效液相色谱同时

检测辣椒粉及辣椒油中苏丹红Ⅰ,Ⅱ,Ⅲ和Ⅳ的方法。该萃取材料对4种苏丹红表现出较强

的萃取能力。样品采用正己烷提取,提取液经固相萃取柱净化,通过清洗除去样品中的天

然色素和油脂干扰,再用乙醇-二氯甲烷(体积比为3∶7)解吸。上述4种苏丹红组分在其质

量浓度为0.05～5 mg/L 的范围内具有良好的线性关系,相关系数的平方均大于0.999;方

法的检出限分别为19.8～28.8 ng/g(辣椒粉)和7.9～11.5 ng/g(辣椒油);日内及日间

相对标准偏差分别小于9.1%和8.8%。在实际样品检测中,4种苏丹红的回收率为82.6%～9

4.0%。结果表明,该方法能较好地去除基质干扰,具有简单、快速、灵敏的特点,适用于食

品中苏丹红的常规分析。

关键词: 腐殖酸, 高效液相色谱, 固相萃取, 苏丹红

Abstract:

Humic acid-bonded silica was prepared and used as solid-phase

extraction material for the pretreatment of Sudan Red dyes in hot chili

products, which was followed by high performance liquid chromatographic

determination. This sorbent exhibits an excellent adsorption capacity for

Sudan Red dyes. A sample was first extracted with n-hexane. Then the

extract was cleaned up by humic acid-bonded silica cartridge and eluted

with ethanol/dichloromethane (3∶7, v/v). Some interferences in hot chili

products such as natural pigments and oil were removed by washing step.

Good linearities were achieved in the range from 0.05 to 5 mg/L for four

Sudan dyes, with linear coefficient r2 values above 0.999. The limits of

detection (LOD) in chili powder and chili oil were from 19.8 to 28.8 ng/g

and 7.9 to 11.5 ng/g， respectively. Excellent method reproducibility was

found by intra- and inter-day precisions (the relative standard

deviations less than 9.1% and 8.8%, respectively). Recoveries for them in

the real samples were between 82.6% and 94.0%. The proposed method is

proved to be simple, rapid, and sensitive in the regular analysis of

Sudan Red Ⅰ, Ⅱ, Ⅲ and Ⅳ in foods.

Key words: high performance liquid chromatography (HPLC), solid-phase extraction (SPE), Sudan Red dyes , humic acid