Determination of paraquat in human blood plasma using reversed-phase ion-pair high-performance liquid chromatography with direct sample injection
Determination of paraquat in human blood plasma using reversed-phase ion-pair high-performance liquid chromatography with direct sample injection
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DOI：
10.1016/s0039-9140(02)00645-8
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发表时间：
2003-04-10
期刊：
影响因子：
6.1
通讯作者：
Burguera, M
中科院分区：
文献类型：
--
作者：
Brunetto, MR;Morales, AR;Burguera, M
本文报道了直接进样反相离子对色谱法测定人血浆样品中百草枯的方法。将血浆滤液直接注射到LiChrospher RP-18烷基二醇二氧化硅（ADS）预柱中，该预柱集成在柱切换系统中，使用3% 2-丙醇和10 mM辛烷磺酸钠（SOS）在0.05 M磷酸盐缓冲液（pH 2.8）中的混合物。用该相洗涤后，用分析移动的相反冲洗ADS预柱，该分析流动相由40%甲醇和10 mM SOS的0.05 M磷酸盐缓冲液组成（pH 2.8），流速为1.0 ml min（-1），以便将分析物携带至常规反相分析柱，在此实现PQ的分离并最终通过UV在258 nm处检测。在9种不同浓度（0.05 - 3.00 μ g PQ ml（-1））下，人血浆样品中PQ的回收率范围为95.0 - 99.5%，变异系数< 2.5%（n = 3）。精密度表示为相对标准偏差为3.5%以下的日间和4.3%以下的日内测量（n = 5）。检测限（信噪比，SN > 3）为0.005 μ g ml（-1），进样体积为200穆尔。所提出的方法是有前途的PQ在低浓度水平的识别和定量，并适用于其分析的人血浆样品从故意或意外中毒的情况下，样品吞吐量为每小时5个样品。(C)2003 Elsevier Science B. V.保留所有权利。
This report describes the determination of paraquat (PQ) in human blood plasma samples by a direct-injection reversed-phase ion-pair chromatographic method. Blood plasma filtrate was injected directly into the LiChrospher(R) RP-18 alkyl-diol silica (ADS) precolumn integrated in a column switching system using a mixture of 3% 2-propanol and 10 mM sodium octane sulfonate (SOS) in a 0.05 M phosphate buffer (pH 2.8). After washing with this phase, the ADS precolumn was back-flushed with the analytical mobile phase consisting of 40% of methanol and 10 mM SOS in a 0.05 M phosphate buffer (pH 2.8) at a flow rate of 1.0 ml min(-1), in order to carry the analyte to a conventional reversed-phase analytical column, where the separation of PQ was achieved and finally detected by UV at 258 nm. The recoveries of PQ from human blood plasma samples ranged between 95.0 and 99.5% at nine different concentrations (from 0.05 to 3.00 mug of PQ ml(-1)) with coefficients of variation < 2.5% (n = 3). The precision expressed as relative standard deviation was below 3.5% for between-day and below 4.3% for within-day measurements (n = 5). The detection limit (signal-to-noise ratio, SN > 3) was 0.005 mug ml(-1) with an injection volume of 200 mul. The proposed method is promising for the identification and quantification of PQ at low concentration levels and is suitable for its analysis in human blood plasma samples from intentional or accidental poisonings cases with a sample throughput of 5 samples per hour. (C) 2003 Elsevier Science B.V. All rights reserved.