Ｏｎ‐Ｌｉｎｅ　ＳＰＥ　ＬＣ／ＡＰＣＩ‐ＭＳ／ＭＳを用いた高感度自動化分析―ヒト血しょう中プラバスタチンおよびその主代謝物の測定法―

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タイトル別名
  • Automated Sensitive Method for Determination of Pravastatin and Its Main Metabolite in Human Plasma by LC/APCI-MS/MS with PROSPEKT-2 On-Line Solid-Phase Extraction
  • On-Line SPE LC/APCI-MS/MSを用いた高感度自動化分析--ヒト血漿中プラバスタチンおよびその主代謝物の測定法
  • On Line SPE LC APCI MS MS オ モチイタ コウカンド ジドウカ ブンセキ ヒト ケッショウ チュウ プラバスタチン オヨビ ソノ シュ タイシャブツ ノ ソクテイホウ
  • —ヒト血漿中プラバスタチンおよびその主代謝物の測定法—

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A method by liquid chromatography/atmospheric pressure chemical ionization tandem mass spectrometry (LC/APCI-MS/MS) for the quantitative determination of pravastatin and its main metabolite (R-416) in human plasma with a fully automated on-line solid-phase extraction (SPE) system, PROSPEKT-2TM was established. The method employed the direct on-line injection of human plasma into the PROSPEKT-2TM system for extraction of the analytes followed by column switching introduction of analytes to the LC/APCI-MS/MS system. The use of on-line SPE system resulted in reducing the sample preparation time and decreasing endogenous interfering substances in the extracts. The lower limit of quantification (LLOQ) for the assay was 0.1 ng/mL for pravastatin and R-416 on a 100 μL plasma sample. The calibration curves were linear for concentrations ranging from 0.1 to 100 ng/mL for both analytes. The intra- and inter-assay precisions were less than 4%. The method provides an automated sample analysis in a total cycle time of 6 min, allowing the analysis of many plasma samples to be conducted with increased throughput and improved robustness.

収録刊行物

  • 質量分析

    質量分析 53 (2), 79-87, 2005

    一般社団法人 日本質量分析学会

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