Quantitative analysis of polyhexamethylene guanidine (PHMG) oligomers via matrix-assisted laser desorption/ionization time-of-flight mass spectrometry with an ionic-liquid matrix.
Quantitative analysis of polyhexamethylene guanidine (PHMG) oligomers via matrix-assisted laser desorption/ionization time-of-flight mass spectrometry with an ionic-liquid matrix.
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DOI：
10.1002/rcm.7096
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发表时间：
2015-01
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影响因子：
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通讯作者：
Donhee Yoon;DongKun Lee;JongHyeon Lee;Sangwon Cha;H. Oh
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文献类型：
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作者：
Donhee Yoon;DongKun Lee;JongHyeon Lee;Sangwon Cha;H. Oh
使用传统结晶基质的基质辅助激光解吸/电离飞行时间质谱仪(MALDI-TOFMS)定量聚合物通常存在样品对样品或样品对样品的重现性差的问题。离子-液体基质已被证明通过提供均匀的样品表面来缓解这些重复性问题，这对于定量聚合物是有用的。在本研究中，我们评估了使用离子液体基质，即1-甲基咪唑α-氰基-4-羟基肉桂酸酯(1-MeIM-CHCA)来量化以液滴形式吸入时对健康造成严重危害的聚六亚甲基胍(PHMG)样品。方法采用包括1-MeIm-CHCA在内的多种离子液体基质，获得PHMG齐聚物的MALDI-TOF质谱图。用不同的多肽内标绘制PHMG齐聚体峰面积与PHMG样品浓度之和的校正曲线。结果与常规结晶基质相比，1-MeIm-CHCA离子液体骨架具有更好的重现性(较低的标准偏差)。此外，通过使用内标肽，可以在至少4个数量级的PMHG浓度范围内获得良好的线性校正曲线。结论以离子液体为基质，以内标物为内标，采用MALDI-TOFMS可以对PHMG样品进行定量表征。
RATIONALE Quantifying polymers by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOFMS) with a conventional crystalline matrix generally suffers from poor sample-to-sample or shot-to-shot reproducibility. An ionic-liquid matrix has been demonstrated to mitigate these reproducibility issues by providing a homogeneous sample surface, which is useful for quantifying polymers. In the present study, we evaluated the use of an ionic liquid matrix, i.e., 1-methylimidazolium α-cyano-4-hydroxycinnamate (1-MeIm-CHCA), to quantify polyhexamethylene guanidine (PHMG) samples that impose a critical health hazard when inhaled in the form of droplets. METHODS MALDI-TOF mass spectra were acquired for PHMG oligomers using a variety of ionic-liquid matrices including 1-MeIm-CHCA. Calibration curves were constructed by plotting the sum of the PHMG oligomer peak areas versus PHMG sample concentration with a variety of peptide internal standards. RESULTS Compared with the conventional crystalline matrix, the 1-MeIm-CHCA ionic-liquid matrix had much better reproducibility (lower standard deviations). Furthermore, by using an internal peptide standard, good linear calibration plots could be obtained over a range of PMHG concentrations of at least 4 orders of magnitude. CONCLUSIONS This study successfully demonstrated that PHMG samples can be quantitatively characterized by MALDI-TOFMS with an ionic-liquid matrix and an internal standard.