...
  • 主题
高级搜索  >
历史搜索 清空历史
首页> 外文期刊>Analytical methods >A fast on-line micro-column sample pretreatment with a HPLC column switching technique and large volume sample injection for determination of non-steroidal anti-inflammatory drugs in human serum
【24h】

A fast on-line micro-column sample pretreatment with a HPLC column switching technique and large volume sample injection for determination of non-steroidal anti-inflammatory drugs in human serum

机译：HPLC柱切换技术和大体积进样的快速在线微柱样品预处理，用于测定人血清中的非甾体类抗炎药

获取原文
           
页面导航
  • 摘要
  • 著录项
  • 相似文献
  • 相关主题

摘要

A fully automated HPLC column-switching method with fast sample pretreatment on a short micro-column was developed for sensitive and quantitative determination of non-steroidal anti-inflammatory drugs (ketoprofen, ibuprofen, sodium diclofenac and flurbiprofen) in human serum with UV detection. The serum samples were diluted 3:1, with 2% acetic acid in acetonitrile, and centrifuged at 4200g for 10 min. 200 ??L of supernatant was injected directly into the HPLC system. An on-line sample clean-up was achieved on a pretreatment micro-column LiChrospher?? RP-18 ADS 25 mm ?— 2.0 mm, 25 ??m (Merck) with a washing mobile phase (acetonitrile:0.085% phosphoric acid; 10:90) at a flow rate of 2.5 mL mina?’1. The valve switch to an analytical column was set at the 7th min in a back-flush mode. Separation of all antiflogistics and internal standard butylparaben was performed using a Chromolith Performance RP 18e 100 ?— 4.6 mm column (Merck) and a mobile phase consisting of 0.085% phosphoric acid and acetonitrile in gradient mode. The column temperature was set at 45 ?°C and a flow rate of 1.0 mL mina?’1 and a UV detector at 210 nm. Standard and matrix calibrations were carried out under the optimal chromatographic conditions in the linearity range 7a€“2000 ng mLa?’1 with good linearity a€“ correlation coefficients for all compounds are in the range 0.9956a€“0.9999, n a‰￥ 6. Limits of quantification were in the range 7a€“56 ng mLa?’1. The accuracy of the method defined as a mean recovery was in the range 81.97a€“118.40%. Intra-day method precision was measured at three concentration levels and relative standard deviations were in the range 0.07a€“1.92%. The developed method showed high sample throughput, fully automated sample clean-up and analysis in time less than 17 min.
机译：开发了一种在短微柱上进行快速样品预处理的全自动HPLC柱切换方法，用于通过UV检测灵敏和定量测定人血清中的非甾体抗炎药（酮洛芬，布洛芬，双氯芬酸钠和氟比洛芬）。用2％的乙腈溶液的乙酸以3：1的比例稀释血清样品，并在4200g下离心10分钟。将200升的上清液直接注入HPLC系统。在预处理的微柱LiChrospher上实现了在线样品净化。 RP-18 ADS 25毫米φ— 2.0毫米，25？m（Merck），流动相为洗涤液（乙腈：0.085％磷酸; 10：90），流速为2.5 mL min-1。在第7分钟以反吹模式将阀切换至分析柱。使用Chromolith Performance RP 18e 100？-4.6 mm色谱柱（Merck）和由0.085％磷酸和乙腈组成的流动相，以梯度模式进行分离所有抗发炎剂和内标对羟基苯甲酸丁酯。柱温设置为45°C，流速为1.0 mL min-1？1，紫外检测器为210 nm。在最佳色谱条件下，在线性范围为7a€“ 2000 ng mLa？'1且线性良好的情况下，进行标准品和基质的校准。所有化合物的相关系数均在0.9956a€0.9999的范围内，n≥6定量限在7a？56 ng mLa？1范围内。定义为平均回收率的方法的准确度在81.97a？118.40％的范围内。在三个浓度水平下测量日内方法的精度，相对标准偏差在0.07a•1.92％的范围内。所开发的方法显示出高的样品通量，全自动样品清洁和分析时间少于17分钟。

著录项

相似文献

  • 外文文献
  • 中文文献
  • 专利
获取原文

客服邮箱：kefu@zhangqiaokeyan.com

京公网安备：11010802029741号 ICP备案号：京ICP备15016152号-6 六维联合信息科技 (北京) 有限公司©版权所有

  • 客服微信

  • 服务号