Quantitation of formate by solid-phase microextraction and gas chromatography--mass spectrometry utilizing a [13C]formate internal standard.

Quantitation of formate by solid-phase microextraction and gas chromatography--mass spectrometry utilizing a [13C]formate internal standard.
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DOI:
10.1016/s0021-9673(02)01996-9
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发表时间:
2003-02
期刊:
Journal of chromatography. A
影响因子:
--
通讯作者:
J. K. Kim;T. Shiraishi;E. Fukusaki;A. Kobayashi
J. K. Kim;T. Shiraishi;E. Fukusaki;A. Kobayashi
中科院分区:
其他
文献类型:
--
作者:
J. K. Kim;T. Shiraishi;E. Fukusaki;A. Kobayashi

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建立了固相微萃取-气相色谱-电子轰击电离质谱(GC-ESI-MS)分析甲酸的新方法。使用[13 C]甲酸作为内标物的该方法,在酯化和纤维吸附步骤期间,[12 C]甲酸/[13 C]甲酸的峰面积比不受不同甲醇或硫酸浓度的影响。相比之下,甲酸/乙腈的峰面积比,如通过常规GC与火焰离子化检测器检测的甲醇或硫酸浓度的影响很大。本方法的甲酸校准曲线在5 - 200 μM范围内具有良好的线性。甲酸浓度的批内和批间测定相对标准偏差均小于1.70%。
A new method for the analysis of formic acid was developed using gas chromatography–electron impact ionization mass spectrometry in the selected ion monitoring mode and solid-phase microextraction. Using this method with [13C]formic acid as an internal standard, the peak area ratio of [12C]formic acid/[13C]formic acid was not affected by differing methanol or sulfuric acid concentrations during the esterification and fiber adsorbing step. In comparison, the peak area ratio of formic acid/acetonitrile as detected by conventional GC with flame ionization detection was greatly affected by methanol or sulfuric acid concentrations. The formic acid calibration curve of our method showed excellent linearity over the range 5 to 200 μM. The within- and between-run assay relative standard deviations for the formic acid concentration were all less than 1.70%.