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首页> 外文期刊>Journal of Pharmaceutical and Biomedical Analysis: An International Journal on All Drug-Related Topics in Pharmaceutical, Biomedical and Clinical Analysis >A novel approach for determination of paraquat based on dried blood spot (DBS) extraction and UHPLC-HRMS analysis
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A novel approach for determination of paraquat based on dried blood spot (DBS) extraction and UHPLC-HRMS analysis

机译:一种基于干血斑(DBS)萃取和UHPLC-HRMS分析的拟法测定百草枯的新方法

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摘要

Paraquat is an effective herbicide chemical but a highly toxic compound for humans and animals. The measurement of paraquat concentration in blood is important to clinic or forensic practice. Herein, a method has been developed for the analysis of paraquat in human blood using dried blood spot (DBS) extraction and subsequent UHPLC-HRMS analysis. Three droplets (100 μL each) of blood were spotted on the Whatman?FTA classic card and then let dry by microwave irradiation (1200?W) for 5?min to prepare DBS. An 8?mm diameter punch was removed from the center of DBS and extracted with 190 μL of mobile phase (20?mM ammonium acetate with 0.1% formic acid and 5% acetonitrile in ultra-pure water) and 10 μL of internal standard (paraquat-d8, 100?ng/mL). After ultrasonic treatment for 10?min, the tube was centrifuged, and the supernatant was then filtered by 0.2 μm membrane and injected into the UHPLC-HRMS system. The method was validated considering the following parameters: selectivity, LOD and LLOQ, linearity, precision, accuracy. The method showed satisfactory linearity in the range of 1–1000?ng/mL, with high determination coefficient (0.9986). LOD was 0.5?ng/mL, and LLOQ was 1?ng/mL. Selectivity, intra and inter day precision and accuracy were acceptable. The validated method was then applied to authentic blood samples and has proved to be a simple, fast and reliable procedure for the determination of paraquat in blood.
机译:百草枯是一种有效的除草剂化学,对人类和动物的一种高毒性化合物。血液中百草浓度的测量对于诊所或法医实践至关重要。这里,已经开发了一种方法,用于使用干血斑(DBS)提取和随后的UHPLC-HRMS分析分析人血液中的百草枯。发现三个液滴(每次100μl)血液在Whatman?FTA经典卡上,然后通过微波辐射(1200→W)干燥5?min以制备DBS。从DBS的中心移除8毫米直径的冲头,用190μl流动相(20μl乙酸铵,乙酸铵20μl乙酸,在超纯水中的5%乙腈)和10μl内标(百草枯-d8,100?ng / ml)。超声处理10≤min后,将管离心,然后将上清液用0.2μm膜过滤并注射到UHPLC-HRMS系统中。考虑以下参数,验证了该方法:选择性,LOD和LLOQ,线性,精度,精度。该方法显示出令人满意的线性度,范围为1-1000μg/ ml,具有高测定系数(0.9986)。 LOD为0.5?ng / ml,LLOQ为1?ng / ml。选择性,内部和日间间精度和准确度是可接受的。然后将验证的方法应用于真实的血液样本,并证明是一种简单,快速可靠的方法,用于测定血液中的百草枯。

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