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采用超高效液相色谱-串联质谱法分析大鼠血浆中的羟化多溴联苯醚。

Analysis of hydroxylated polybrominated diphenyl ethers in rat plasma by using ultra performance liquid chromatography-tandem mass spectrometry.

机构信息

Department of Chemistry, Hong Kong Baptist University, Hong Kong SAR, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 May 1;879(15-16):1086-90. doi: 10.1016/j.jchromb.2011.03.024. Epub 2011 Mar 21.

Abstract

Ultra performance liquid chromatography (UPLC) provides improved resolution, speed and sensitivity compared to conventional high performance liquid chromatography (HPLC). In this study, a robust UPLC-ESI-MS/MS method was developed for the rapid determination of nine hydroxylated polybrominated diphenyl ethers (OH-PBDEs) in rat plasma. Under the optimized conditions, the OH-PBDE congeners were eluted within 7.0 min. The limits of quantification defined at the signal-to-noise ratio of 10 were 0.17-2.78 ng/mL in rat plasma. The method provided good linearity for the calibration curves with recoveries of 93.3-114.0% and repeatability with relative standard deviation (RSD) of 0.6-5.8% for intra-day and 3.2-10.4% for inter-day measurements. The developed method was applied for supporting the pharmacokinetics investigation of 6-OH-BDE-47 in two groups of Sprague-Dawley rats that received, respectively a single dose of 0.60 mg/kg (high dose) and 0.15 mg/kg (low dose) by intravenous injection. The results showed that plasma levels of 6-OH-BDE-47 declined bi-exponentially with elimination half-life of 71.7 and 85.6 min for lower and higher dose group, respectively. The obtained results of short elimination half-life suggested that 6-OH-BDE-47 might not accumulate significantly in rat.

摘要

超高效液相色谱 (UPLC) 与传统高效液相色谱 (HPLC) 相比,具有更高的分辨率、速度和灵敏度。本研究建立了一种快速测定大鼠血浆中 9 种羟基多溴二苯醚 (OH-PBDEs) 的 UPLC-ESI-MS/MS 方法。在优化条件下,OH-PBDE 同系物在 7.0 min 内洗脱。在信噪比为 10 时,大鼠血浆中 OH-PBDE 同系物的定量限为 0.17-2.78 ng/mL。该方法的校准曲线线性良好,日内和日间测定的回收率为 93.3-114.0%,相对标准偏差 (RSD) 为 0.6-5.8%和 3.2-10.4%。该方法用于支持静脉注射 0.60 mg/kg(高剂量)和 0.15 mg/kg(低剂量)两种剂量组的 Sprague-Dawley 大鼠 6-OH-BDE-47 的药代动力学研究。结果表明,低剂量和高剂量组大鼠血浆中 6-OH-BDE-47 呈双指数衰减,消除半衰期分别为 71.7 和 85.6 min。较短的消除半衰期表明 6-OH-BDE-47 可能不会在大鼠体内显著蓄积。

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