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Determination of cocaine/crack biomarkers in colostrum by LC-MS following protein precipitation

机译:蛋白质沉淀后LC-MS法测定初乳中的可卡因/裂纹生物标志物

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摘要

Drug abuse by nursing mothers is an ongoing concern because it may cause many adverse effects to the newborns. The development of analytical methods to analyze drugs of abuse in colostrum (first milk produced after birth) has a huge importance, because it enables the monitoring and the correct follow-up to users and newborns. A liquid chromatography mass spectrometry (LC-MS) method was developed and validated for the determination of cocaine and smoked cocaine (crack) biomarkers in colostrum. Cocaine (COC) and its major metabolite benzoylecgonine (BZE), the pyrolytic products anhydroecgonine methyl ester (AEME) and anhydroecgonine (AEC) were analyzed after a simple protein precipitation procedure using atropine (ATP) as internal standard (IS). Applying a chemometric approach study, all peaks were chromatographically separated at isocratic condition with a Kinetex HILIC column for polar compounds, at 30 degrees C in 12 min. One ion was detected for the quantification and three ions for confirmation of each analyte. The method was linear for all analytes in the concentration range of 5-300 ng/mL with correlation coefficients (r) between 0.9983 and 0.9996. The lower limit of quantification (LLOQ) was 5 ng/mL with acceptable validation-parameters. Matrix effect was assessed by post-extraction addition-approach and showed good results, demonstrating that protein precipitation cleaning procedure is fast, reliable and demand small quantities of organic solvent. The LC-MS method is fast and cheap compared to other equipments and was also successfully applied to assess real samples of colostrum from nursing mothers who were suspect of cocaine/crack abuse. (C) 2014 Elsevier B.V. All rights reserved.
机译:哺乳母亲滥用药物一直是一个令人担忧的问题,因为它可能对新生儿造成许多不利影响。开发用于分析初乳中滥用药物(出生后产生的第一批牛奶)的分析方法非常重要,因为它可以监控使用者和新生儿,并对他们进行正确的跟进。建立了液相色谱质谱(LC-MS)方法,并验证了该方法可用于测定初乳中的可卡因和烟熏可卡因(裂纹)生物标志物。使用阿托品(ATP)作为内标(IS)进行简单的蛋白质沉淀后,分析了可卡因(COC)及其主要代谢物苯甲酰芽子碱(BZE),热解产物脱水芽子碱甲酯(AEME)和脱水芽子碱(AEC)。应用化学计量学方法研究,所有色谱峰均通过Kinetex HILIC色谱柱在30摄氏度下于12分钟内在等度条件下色谱分离。检测到一个离子进行定量,并检测了三个离子以确认每种分析物。该方法对于浓度范围为5-300 ng / mL的所有分析物都是线性的,相关系数(r)在0.9983至0.9996之间。定量下限(LLOQ)为5 ng / mL,验证参数可接受。通过萃取后添加方法评估基质效果,并显示出良好的结果,表明蛋白质沉淀清洗程序快速,可靠且需要少量有机溶剂。与其他设备相比,LC-MS方法既快速又便宜,并且还成功地用于评估怀疑可卡因/龟裂滥用的哺乳母亲的初乳样品。 (C)2014 Elsevier B.V.保留所有权利。

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