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  

Detection of glucocorticoids by pressurized capillary electrochromatography with ultra-violet detection and its application in hair analysis

作　　者：李博祥 郑敏敏 卢兰香 吴晓苹[1] 

机构地区：[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

出　　处：《色谱》2011年第8期798-804,共7页Chinese Journal of Chromatography

基　　金：国家自然科学基金项目(21075017)

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pH8.0,1.5mmol/L的Tris-乙腈(65∶35,v/v),检测波长为245nm、分离电压为-10kV、反压为10.5MPa、泵流速为0.05mL/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20min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。An effective and convenient method for glucocorticoid analysis in hair by reversed-phase pressurized capillary electrochromatography（pCEC） with ultra-violet（UV） detection was developed.Eight glucocorticoids（betamethasone,dexamethasone,prednisone,prednisolone,prednisolone acetate,hydrocortisone acetate,cortisone acetate and corticosterone） were separated within 20 min in an isocratic mode pCEC.The separations were performed on a reversed-phase C18 column,and with 245 nm as the UV detection wavelength.The mobile phase was composed of 1.5 mmol/L Tris buffer（pH 8.0） and acetonitrile（65∶35,v/v）,at a pump flow rate of 0.05 mL/min.All of the compounds showed good linearity in the range of 0.036-4.0 mmol/L.The limits of detection（LODs） for all glucocorticoids were of μg/g levels.The proposed method was applied to the analysis of hair samples.The interference of hair matrices was effectively eliminated by protein enzymatic digestion,followed by a methanol extraction and a solid phase extraction（SPE） clean up step.The average recoveries of 71%-85% at different fortified levels of glucocorticoids were achieved.This non-invasive method is useful for rapidly estimating the level of drug exposure in drug chronic abuse and monitoring the compliance of therapeutic drugs.

关 键 词：加压毛细管电色谱 紫外检测 糖皮质激素 头发 

分 类 号：O658[理学—分析化学]