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An ultra high performance liquid chromatography-tandem mass spectrometry method for the quantification of linagliptin in human plasma

机译：一种超高效液相色谱 - 串联质谱法，用于量子血浆Linagliptin定量

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摘要

A simple, rapid, sensitive, reliable and selective ultra high performance liquid chromatography (UHPLC)-tandem mass spectrometry (MS/MS) method was developed for the quantification of linagliptin (LGN) in human plasma. LGN and its deuterated internal standard (IS) LGN-d4 were extracted from a low-plasma sample (volume: 300 mu L) by a simple liquid-liquid extraction protocol. Efficient estimation of the analyte and IS at a mean retention time (RT) of 1.75 and 1.74 min respectively, with a rapid 3.5 min run time per sample was chromatographically established on a Gemini C18 (100 mm x 4.6 mm, 3 mu) column under simple isocratic elution conditions, using a mixture of 10 mM ammonium formate : methanol [20 : 80 (v/v)] delivered at a flow rate of 0.5 mL min(-1). Following the separation of the compounds, protonated precursor -> product ion transitions were monitored for LGN (m/z: 473.3 -> 420.1) and IS (m/z: 477.5 -> 424.3) on a triple quadrupole mass spectrometer, operating in a multiple reaction monitoring (MRM) mode. The most recent regulatory guidelines were adopted during the method validation. The method demonstrated very good analyte and IS recovery (not less than 71.0%), precision (<= 8.6% CV), accuracy (range: 86.7% to 95.6%) and linearity (r > 0.99) across a clinically relevant LGN plasma concentration range: 50.3 to 12 115.5 pg mL(-1). The validated method was successfully applied to pharmacokinetic study samples for measuring linagliptin plasma levels.
机译：开发了一种简单，快速，灵敏，可靠和选择性的超高效液相色谱（UHPLC） - 用于量子血浆中Linagliptin（LGN）的定量Linagliptin（LGN）的质谱（MS / MS / MS）方法。通过简单的液 - 液萃取方案从低血浆样品（体积：300μl）中提取LGN及其氘代的内标（IS）LGN-D4。分析物的有效估计分别为1.75和1.74分钟的平均保留时间（RT），在Gemini C18（100mm×4.6mm，3μm）柱上进行色谱自动建立3.5分钟的3.5分钟运行时间简单的等家谱洗脱条件，使用10mM甲酸铵的混合物：甲醇[20：80（v）]以0.5mL min（-1）的流速递送。在分离化合物之后，监测质子化前体 - >对LGN（M / Z：473.3-> 420.1）监测产物离子转变，在三重四极杆质谱仪上（M / Z：477.5-> 424.3），在a中运行多重反应监测（MRM）模式。在方法验证过程中采用了最新的监管指南。该方法证明了非常好的分析物，恢复（不小于71.0％），精度（<= 8.6％CV），精度（范围：86.7％至95.6％）和线性度（r> 0.99），临床相关的LGN等离子体浓度范围：50.3至12 115.5 pg ml（-1）。经过验证的方法已成功应用于用于测量Linagliptin等离子体水平的药代动力学研究样品。

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  • 来源
    《RSC Advances》 |2016年第71期|共11页
  • 作者

    Nannapaneni Nagaraj Kumar; Jalalpure Sunil S.; Muppavarapu Rajendraprasad; Sirigiri Sunil Kumar;

  • 作者单位

    KLE Univ KLE Coll Pharm Dr Prabhakar Kore Basic Sci Res Ctr Belagavi 590010 Karnataka India;

    KLE Univ KLE Coll Pharm Dr Prabhakar Kore Basic Sci Res Ctr Belagavi 590010 Karnataka India;

    Jeevan Sci Technol Ltd Bioanalyt Res Unit Hyderabad 500008 Andhra Pradesh India;

    Jeevan Sci Technol Ltd Bioanalyt Res Unit Hyderabad 500008 Andhra Pradesh India;

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