Laser desorption Fourier transform ion cyclotron resonance mass spectrometry vs. fast atom bombardment magnetic sector mass spectrometry for drug analysis.
Laser desorption Fourier transform ion cyclotron resonance mass spectrometry vs. fast atom bombardment magnetic sector mass spectrometry for drug analysis.
复制标题
用于药物分析的激光解吸傅里叶变换离子回旋共振质谱与快原子轰击扇形磁质谱。
DOI：
10.1021/ac00291a043
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发表时间：
1985
影响因子：
7.4
通讯作者：
Weisenberger,CR
中科院分区：
文献类型：
--
作者：
Shomo2nd,RE;Marshall,AG;Weisenberger,CR
本文用双聚焦扇形磁共振快原子轰击和脉冲CO_2激光解吸电离傅里叶变换离子回旋共振质谱法测定了几种低挥发性药物（阿莫西林，mol wt 365;柔红霉素，mol wt 527;红霉素，mol wt 733;地高辛，mol wt 780）的质谱。与FAB/MS相比，由单个激光脉冲产生的LD/FT/ICR光谱产生更突出的分子或伪分子离子，几乎没有碎片。另外的主要碎片峰（如果需要）可以通过来自同一激光器（LD/EI/FT/ICR）的第二脉冲产生的中性粒子的电子电离来产生。四组分混合物的LD/FT/ICR质量校准在404< m/z<819的质量范围内产生优于5 ppm的质量精度。直到最近，不挥发性物质的质谱是通过首先蒸发样品，然后电离（通常通过电子束的电子电离（El））两个不同的步骤获得的。几种较新的方案在一个过程中实现了解吸和电离：场解吸（1），等离子体解吸（2），二次离子质谱（3，4），激光解吸（5），和（液体）快原子轰击（FAB）（6）和热喷雾（7）。其中，FAB已成为最普遍的流行，因为样品制备的容易和操作简单。不久之后，Kistemaker等人。(5)证明了激光解吸/电离可以从有机大分子中产生分子或准分子离子，测试了各种激光/质谱仪配置。从许多这样的实验，现在看来，几乎任何脉冲激光能够产生约。10 MW/cm 2的功率入射到金属探针上的固体或溶剂蒸发样品上可以产生定性相似的结果（8-10）。最常见的质谱仪选择是飞行时间设计（10），因为大多数其他质谱仪无法在激光脉冲后的可用时间内扫描必要的质量范围。不幸的是，即使是最好的飞行时间仪器在最需要激光源的质量范围（500< mfq< 5000）内也提供相对较差的质量分辨率（11）。傅里叶变换离子回旋共振质谱仪（FT/ICR或FT/MS）（12，13）提供了高质量分辨率和快速的数据采集的整个频谱一次（14，15），本质上是一个脉冲实验。因此，它非常适合激光解吸质谱（LD/MS）。一旦实验的可行性得到证明（8-10），LD/FT/ICR技术就由Hein和Cody发展到了目前的状态（16），并迅速被其他人应用（14，15，17，18）。在本文中，我们提出了第一个
Mass spectra of severalclinically Important drugs of low volatility (amoxicillin, mol wt 365; daunorubicin, mol wt 527; erythromycin, mol wt 733; digoxin, mol wt 780) have been obtained via fast atom bombardment with a double-focusing magnetic sector Instrument and via pulsed C02 laser desorption Ionization Fourier transform ion cyclotron resonance mass spectrometry. Compared to FAB/MS, the LD/FT/ICR spectrum resulting from a single laser pulse produces a much more prominent molecular or pseudomolecular ion with little fragmentation. Additional major fragment peaks (If desired) can be produced by electron Ionization of the neutrals pro-duced by a second pulse from the same laser (LD/EI/FT/ICR). LD/FT/ICR mass calibration for a four-component mixture yields a mass accuracy of better than 5 ppm over a mass range of 404< m/z< 819.Until relatively recently, mass spectra of involatile substances were obtained by first vaporizing the sample and then ionizing it (usually via electron ionization (El) with an electron beam) in two distinct steps. Several newer schemes achieve desorption and ionization in a single procedure: field de-sorption (1), plasmadesorption (2), secondary ion mass spectrometry (3, 4), laser desorption (5), and (forliquids) fast atom bombardment (FAB)(6) and thermospray (7). Of these, FAB has become the most generally popular because of the ease of sample preparation and simplicity of operation. Soon after Kistemaker et al.(5) demonstrated that laser desorption/ionization couldproduce molecular or pseudo-molecular ions from large organic molecules, various laser/mass spectrometer configurations were tested. From a number of such experiments, it now appears that virtually any pulsed laser able to generate ca. 10 MW/cm2 of power incident on a solid or solvent-evaporated sample on a metal probe can yield qualitatively similar results (8-10). The most common mass spectrometer choicehas been the time-of-fiight design (10), because mostother mass spectrometers cannot scan the necessary mass range in the time available following the laser pulse. Unfortunately, even the best time-of-flight instruments offer relatively poor mass resolution in the mass range (500< mfq< 5000) for which the laser source is most needed (11). Fourier transform ion cyclotron resonance mass spectrom-etry (FT/ICR or FT/MS)(12, 13) offers high mass resolution and rapid data acquisition of the whole spectrum at once (14, 15) and is inherently a pulsed experiment. It is thus ideally suited for laser desorption mass spectrometry (LD/MS). Once the feasibility of the experiment had been demonstrated (8-10), the LD/FT/ICR technique was developed to its present state by Hein and Cody (16), and promptly applied by others (14, 15, 17, 18). In this paper, we present the first