分析仪器
分析儀器
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ANALYTICAL INSTRUMENTATION
2013年
5期
65-75
,共11页
胶束毛细管电泳%二极管阵列检测%β-兴奋剂
膠束毛細管電泳%二極管陣列檢測%β-興奮劑
효속모세관전영%이겁관진렬검측%β-흥강제
micellar electrokinetic capillary chromatography (MECC)%diode array detector (DAD)%β-agonists
建立了胶束毛细管电泳分离结合二极管阵列(DAD )检测“瘦肉精”的方法。以10 mmol/L 硼酸盐(Na2B4O7-NaOH)(pH10.5)为背景电解质,同时加入10 mmol/L表面活性剂十二烷基硫酸钠(SDS)组成电泳运行缓冲液,分离和定量检测沙丁胺醇(Salbutamol ,SAL)、特步他林(Terbutaline ,TER)、西马特罗(Cimaterol ,CIM )、莱克多巴胺(Ractopamine ,RAC)和克伦特罗(Clenbuterol ,CLB)5种“瘦肉精”类药物(β-兴奋剂)。考察了运行缓冲液的浓度和pH值、表面活性剂浓度、分离电压和毛细管柱温度等因素对分离和检测的影响并进行了优化。在最佳条件下,5种药物在14 min内可实现良好的基线分离,检测限(S/N>3)均低于0.2μg/mL。以尿液样品为例进行了生物样品的初步检测,其回收率均高于97%,方法快速、简便、可靠。
建立瞭膠束毛細管電泳分離結閤二極管陣列(DAD )檢測“瘦肉精”的方法。以10 mmol/L 硼痠鹽(Na2B4O7-NaOH)(pH10.5)為揹景電解質,同時加入10 mmol/L錶麵活性劑十二烷基硫痠鈉(SDS)組成電泳運行緩遲液,分離和定量檢測沙丁胺醇(Salbutamol ,SAL)、特步他林(Terbutaline ,TER)、西馬特囉(Cimaterol ,CIM )、萊剋多巴胺(Ractopamine ,RAC)和剋倫特囉(Clenbuterol ,CLB)5種“瘦肉精”類藥物(β-興奮劑)。攷察瞭運行緩遲液的濃度和pH值、錶麵活性劑濃度、分離電壓和毛細管柱溫度等因素對分離和檢測的影響併進行瞭優化。在最佳條件下,5種藥物在14 min內可實現良好的基線分離,檢測限(S/N>3)均低于0.2μg/mL。以尿液樣品為例進行瞭生物樣品的初步檢測,其迴收率均高于97%,方法快速、簡便、可靠。
건립료효속모세관전영분리결합이겁관진렬(DAD )검측“수육정”적방법。이10 mmol/L 붕산염(Na2B4O7-NaOH)(pH10.5)위배경전해질,동시가입10 mmol/L표면활성제십이완기류산납(SDS)조성전영운행완충액,분리화정량검측사정알순(Salbutamol ,SAL)、특보타림(Terbutaline ,TER)、서마특라(Cimaterol ,CIM )、래극다파알(Ractopamine ,RAC)화극륜특라(Clenbuterol ,CLB)5충“수육정”류약물(β-흥강제)。고찰료운행완충액적농도화pH치、표면활성제농도、분리전압화모세관주온도등인소대분리화검측적영향병진행료우화。재최가조건하,5충약물재14 min내가실현량호적기선분리,검측한(S/N>3)균저우0.2μg/mL。이뇨액양품위례진행료생물양품적초보검측,기회수솔균고우97%,방법쾌속、간편、가고。
A rapid ,simple and reliable micellar electrokinetic capillary chromatography (M ECC) elec-troseparation method coupled with DAD (diode array detector)detection was developed for the analysis of β-agonists. Fiveβ-agonists :Salbutamol(SAL) ,Terbutaline(TER) ,Cimaterol(CIM ) ,Ractopamine(RAC) and Clenbuterol(CLB) were separated and quantitatively detected using a background electrolyte consisting of 10 mmol/L borate(Na2B4 O7-NaOH) (pH 10.5) with 10 mmol/L sodium dodecyl sulfate. Factors influ-encing the separation and detection such as concentration and pH value of the running buffer ,surfactants , separation electrical voltage and column temperature were investigated and optimized. Under the optimum conditions ,the baseline separation of the five selected compounds was achieved within 14 min and limits of detection(S/N>3) lower than 0.2 μg/mL. With this measure ,fiveβ-agonists in urine samples were suc-cessfully determined with the recovery more than 97%.