Development and validation of a highly sensitive LC–MS/MS method for the determination of acacetin in human plasma and its application to a protein binding study

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• 作者：Sang-Bum Kim ; Taehun Lee ; Hun Seok Lee ; Chung Kil Song…
• 关键词：Acacetin ; LC–MS/MS ; Human plasma ; Protein binding
• 刊名：Archives of Pharmacal Research
• 出版年：2016
• 出版时间：February 2016
• 年：2016
• 卷：39
• 期：2
• 页码：213-220
• 全文大小：888 KB
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• 作者单位：Sang-Bum Kim (1)
  Taehun Lee (2)
  Hun Seok Lee (2)
  Chung Kil Song (3)
  Hyun-Jong Cho (4)
  Dae-Duk Kim (2)
  Han-Joo Maeng (5)
  In-Soo Yoon (6)
  
  1. New Drug Development Center, Daegu–Gyeongbuk Medical Innovation Foundation, Daegu, 701-310, Republic of Korea
  2. College of Pharmacy and Research Institute of Pharmaceutical Sciences, Seoul National University, Seoul, 151-742, Republic of Korea
  3. Institute of Nanoscience and Technology, Hanyang University, Seoul, 133-791, Republic of Korea
  4. College of Pharmacy, Kangwon National University, Chuncheon, 200-701, Republic of Korea
  5. College of Pharmacy, Gachon University, 191 Hambakmoei-ro, Yeonsu-gu, Incheon, 406-799, Republic of Korea
  6. College of Pharmacy and Natural Medicine Research Institute, Mokpo National University, 1666 Youngsan-ro, Muan-gun, Jeonnam, 534-729, Republic of Korea
  
• 刊物主题：Pharmacy; Pharmacology/Toxicology;
• 出版者：Springer Netherlands
• ISSN：1976-3786

文摘

A highly sensitive bioanalytical method for the quantification of acacetin in human plasma was developed and comprehensively validated using liquid chromatography-tandem mass spectrometry (LC–MS/MS). A minimal volume of human plasma sample (20 μL) was prepared by simple deproteinization with 80 μL of acetonitrile. Chromatographic separation was performed using Kinetex C₁₈ column with an isocratic mobile phase consisting of water and acetonitrile (20:80, v/v) containing 0.1 % formic acid at a flow rate of 0.3 mL/min over a total run time of 2.0 min. Mass spectrometric detection was performed using multiple reaction-monitoring modes at the mass/charge transitions m/z 285.22 → 242.17 for acacetin and m/z 277.59 → 175.04 for chlorpropamide (internal standard). The calibration curve was linear over the range of 0.1–500 ng/mL with a lower limit of quantitation of 0.1 ng/mL. The coefficients of variation for both intra- and inter-day validation were less than 11.9 %, and the intra- and inter-day accuracy ranged from 96.8 to 108 %. Mean recovery of acacetin in human plasma was within the range of 91.5–95.6 %. This validated LC–MS/MS method was successfully applied to a human plasma protein binding study that indicated extensive and concentration-independent protein binding of acacetin in human plasma.