色谱

色谱

• 研究论文 • 上一篇    

加压毛细管电色谱—紫外检测法分析糖皮质激素及其在头发检测中的应用

李博祥, 郑敏敏, 卢兰香, 吴晓苹*   

  1. 食品安全分析与检测技术教育部重点实验室, 福州大学化学化工学院, 福建 福州 350108
  • 收稿日期:2011-04-14 修回日期:2011-05-02 出版日期:2011-08-28 发布日期:2011-09-28
  • 通讯作者: 吴晓苹,博士,教授,主要从事分析化学、食品安全与环境分析研究
  • 基金资助:

    国家自然科学基金项目(21075017)

Analysis of glucocorticoids in hair by pressurized capillary electrochromatography with ultra-violet detection

LI Boxiang, ZHENG Minmin, LU Lanxiang, WU Xiaoping*   

  1. Key Laboratory of Analysis and Detection Technology for Food Safety, Ministry of Education, College of Chemistry and Chemical Engineering, Fuzhou University, Fuzhou 350108, China
  • Received:2011-04-14 Revised:2011-05-02 Online:2011-08-28 Published:2011-09-28

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摘要： 采用反相加压毛细管电色谱与紫外检测联用技术,建立了一种高效、简便的糖皮质激素分析方法,适用于头发中糖皮质激素的检测。使用C18反相色谱柱,流动相为pH 8.0, 1.5 mmol/L的Tris-乙腈(65:35, v/v),检测波长为245 nm、分离电压为~10 kV、反压为10.5 MPa、泵流速为0.05 mL/min,进行等度洗脱,倍他米松、地塞米松、泼尼松、泼尼松龙、醋酸泼尼松龙、醋酸氢化可的松、醋酸可的松、皮质脂酮等8种激素在20 min内实现快速分离。各组分的质量浓度线性范围达到3个数量级,检出限(S/N=3)在μg/g水平,迁移时间和峰面积的相对标准偏差(RSD)分别小于4.8%和7.4%。将所建立方法应用于头发样品分析,检测前采用蛋白酶水解提取和净化处理样品,不同浓度糖皮质激素的回收率为71%～85%。该研究为糖皮质激素药物暴露监测以及压力检测提供了新手段,有望用于滥用药物的控制和临床诊断。

关键词: 加压毛细管电色谱, 糖皮质激素, 头发, 紫外检测

Abstract: This study describes an effective and convenient method for the separation and determination of the glucocorticoids residues in hair. Compared to most reported methods of high performance liquid chromatography using gradient elution，this analysis is performed utilizing isocratic elution reversd-phase pressurized capillary electrochromatography with UV detection. Eight glucocorticoids (betamethasone, dexamethasone, prednisone, prednisolone, prednisolone acetate, hydrocortisone acetate, cortisone acetate and corticosterone) are separated within 20min on a reversed-phase C18 column, with the Tris buffer (pH 8, 1.5 mM)– acetonitrile (65:35, v/v) as mobile phase and 245nm as the UV detection wavelength, and the flow rate of pump is 0.05 mL/min. All the compounds show good linearity in the concentration range of analysis. Detection limits (LODs) for all glucocorticoids are of 10-6 mol/L levels. The proposed method is applied to the analysis of hair samples. The interference of hair matrices were effectively eliminated by enzymatic digestion followed by a methanol extraction and a solid phase extraction (SPE) clean up step. Average recoveries of 71–85% at different fortified levels of glucocorticoids are achieved. This non-invasive method is useful for rapidly estimating the level of drug exposure in drug abuse and monitoring the compliance of therapeutic drugs.

Key words: glucocorticoids, hair testing, pressurized capillary electrochromatography, UV detection