高效液相色谱-质谱法测定棉籽仁中左旋和右旋棉酚含量

姚军; 何晓文; 李新霞; 张煌涛; 鹿毅

doi:10.13386/j.issn1002-0306.2013.19.030

高效液相色谱-质谱法测定棉籽仁中左旋和右旋棉酚含量

1. 新疆医科大学药学院
2. 新疆产品质量监督检验研究院

基金项目:

国家自然科学基金项目(31160322)；

详细信息

作者简介:
姚军 (1973-) , 男, 博士, 副教授, 研究方向:食品及药品质量控制技术研究。;

中图分类号: TS207.3;O657.63
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出版历程
- 收稿日期: 2013-02-19

Determination of (-) -and (+) -gossypol in cottonseed by high-performance liquid chromatography with mass spectrum

College of Pharmacy, Xinjiang Medical University
Xinjiang Provincial Supervising and Testing Research Institute for Products Quality

摘要

摘要: 建立一种高效液相色谱-质谱法测定棉籽仁中（-）-棉酚和（+）-棉酚含量的检测方法。样品经石油醚脱脂,含10%冰醋酸的N,N-二甲基甲酰胺超声波提取,以（R）-（-）-2-胺基-1-丙醇为手性拆分试剂进行柱前衍生化反应,乙腈∶1.0%甲酸=85∶15作为流动相,用Agilent XDB-C18色谱柱（250mm×4.6mm,5μm）分离,流速1mL/min,柱后分流比15%,在电喷雾正离子模式下对m/z 633.2进行选择性离子监测。该方法下棉酚在1.93³8.6μg/mL范围内线性关系良好,（-）-和（+）-棉酚在低、中、高的三个添加水平范围内的平均回收率为99.4%¹03.0%,RSD值为1.27%³.86%;（-）-和（+）-棉酚的检出限分别为2.52、3.41ng/mL,定量限分别为8.39、11.4ng/mL。结果表明,此法操作简便、快速、灵敏、准确,样品处理简便易行,适于测定棉籽仁中（-）和（+）-棉酚的含量。
- 高效液相色谱-质谱法（HPLC-MS） /
- 棉籽仁 /
- (-)-棉酚 /
- (+)-棉酚 /
- (R)-（-）-2-胺基-1-丙醇
Abstract: A HPLC with mass spectrum derivatization method was developed for the determination of (-) -and (+) -gossypol in cottonseed.After degreased by petroleum ether, the samples were extracted with ultrasoninc by 10% glacial acetic acid of N, N-dimethyl formamide formamide and (R) - (-) -2-amino-1-propanol was selected as the chiral separation reagent.Then the chromatographic separation was carried out on an Agilent XDB-C 18 column (250mm ×4.6mm, 5μm) with a mobile phase consisted of 85% acetonitrile and 15% water within 1.0% formic acid at a flow rate of 1mL /min.The condition of mass spectrometer was operated at m /z 633.2 in positive elctrospray ionization mode.It showed that a good linear relationship between HPLC peak area and gossypol concentration was obtained over the range of 1.93³8.6μg /mL, mean spike recoveries of (-) -and (+) -gossypol at three levels were 99.4% ¹03.0%, with RSD ranged from 1.27% ³.86%.The limits of detection were 2.52ng /mL and 3.41ng /mL, while the limits of quantification were 8.39ng /mL and 11.4ng /mL for (-) -and (+) -gossypol respectively.The method provided simplicity, rapidity, sensitivity and accuracy, and therefore was applicable to the determination of (-) and (+) -gossypol in cottonseed.
- HPLC-MS /
- cottonseed /
- (-) -gossypol /
- (+) -gossypol /
- (R) - (-) -2-Amino-1-propanol

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参考文献(20)

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