食品科学

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柱前手性衍生化-高效液相色谱法测定棉籽仁中左旋和右旋棉酚含量

何晓文,李新霞,姚 军,张煌涛,薛海燕   

  1. 1.新疆医科大学药学院,新疆 乌鲁木齐 830054;2.新疆产品质量监督检验研究院,新疆 乌鲁木齐 830054
  • 出版日期:2013-06-25 发布日期:2013-06-17

Determination of (-) and (+)-Gossypols in Cottonseed Kernel by High-Performance Liquid Chromatography with Chiral Pre-column Derivatization

HE Xiao-wen,LI Xin-xia,YAO Jun,ZHANG Huang-tao,XUE Hai-yan   

  1. 1. College of Pharmacy, Xinjiang Medical University, Ürümqi 830054, China;
    2. Xinjiang Provincial Supervising and Testing Research Institute for Products Quality, Ürümqi 830054, China
  • Online:2013-06-25 Published:2013-06-17

摘要:

目的:建立柱前手性衍生化-高校液相色谱法测定棉籽仁中(-)-棉酚和(+)-棉酚含量的检测方法。方法:采用XDB-C18色谱柱(250mm×4.6mm,5μm),流动相为乙腈-10mmol/L KH2PO4缓冲溶液(磷酸调pH3.0)(80:20,V/V),(R)-(-)-2-胺基-1-丙醇为手性拆分试剂,流速1.0mL/min,柱温40℃,检测波长247nm。结果:(-)-棉酚在1.96~29.46μg/mL质量浓度范围内线性关系良好,回收率为99.7%~104.1%,RSD值为1.50%~3.07%;(+)-棉酚在1.82~27.30μg/mL质量浓度范围内线性关系良好,回收率为100.6%~105.8%,RSD值为1.08%~3.53%。结论:此法操作简便、快速、灵敏、准确,样品处理简便易行,可用于棉籽仁及相关食品中(-)-和(+)-棉酚的含量检测。

关键词: 棉籽仁, (-)-棉酚, (+)-棉酚, (R)-(-)-2-胺基-1-丙醇, 柱前手性衍生化, 高效液相色谱法

Abstract:

An HPLC with chiral pre-column derivatization method was developed for the determination of (-)-and
(+)-gossypols in cottonseed kernel. Chromatographic separation was carried out on an Agilent XDB-C18 column (250
mm × 4.6 mm, 5 μm) with a mobile phase which consisted of 80% acetonitrile and 20% 10 mmol/L KH2PO4 buffer adjusted
to pH 3.0 with H3PO4 at a flow rate of 1.0 mL/min. (R)-(-)-2-amino-1-propanol was used as a chiral separation reagent
and the detection wavelength was set at 247 nm. A good linear relationship between HPLC peak area and (-)-gossypol
concentration was obtained over the range of 1.96 to 29.46 μg/mL, and the mean recoveries of (-)-gossypol at three spiked
levels were 99.7% -104.1%, with RSDs rangeing from 1.50% to 3.07%. As for (+)-gossypol, the linear range was 1.82-
27.30 μg/mL, mean recoveries at three spiked levels were 100.6%-105.8% with RSDs ranging from 1.08% to 3.53%. The
method provides simplicity, rapidity, sensitivity and accuracy, and therefore is applicable to the determination of (-)-and
(+)-gossypols in cottonseed kernel and related foods.

Key words: cottonseed, (-)-gossypol, (+)-gossypol, (R)-(-)-2-amino-1-propano, chiral pre-column derivatization, high performance liquid chromatography (HPLC)