Development of in-tube solid-phase microextraction/liquid chromatography/electrospray ionization mass spectrometry for the analysis of mutagenic heterocyclic amines
Development of in-tube solid-phase microextraction/liquid chromatography/electrospray ionization mass spectrometry for the analysis of mutagenic heterocyclic amines
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DOI：
10.1007/bf02493657
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发表时间：
1999-11-01
期刊：
影响因子：
1.7
通讯作者：
Pawliszyn, J
中科院分区：
文献类型：
--
作者：
Kataoka, H;Pawliszyn, J
管内固相微萃取（管内 SPME）与液相色谱/电喷雾电离质谱 (LC/ESI-MS) 相结合，用于分析诱变杂环胺。杂环胺的 LC/MS 分析最初是通过将液体注射到 LC 柱上进行的。本研究中测试的所有杂环胺都给出了非常简单的 ESI 质谱，并且对于除 Glu-P-1 和 Glu-P-2 之外的所有杂环胺都观察到了与 [M + H](+) 相对应的强信号（从这些胺中观察到 [M + NH(4) - H(2)O](+) 离子）。除始终共洗脱的 A alpha C 和 Glu-P-2 外，所有杂环胺均可使用 Supelcosil LC-CN 柱很好地分离。为了优化杂环胺的萃取，使用五种代表性化合物检查了几个管内固相微萃取参数。最佳提取条件如下：使用Omekawax 250毛细管柱，以100 μL min(-1)的流速，将30 μL样品在100 mM Tris-HCl (pH 8.5)中进行10次吸取/分配步骤。毛细管柱提取的杂环胺在进样前吸入30μL甲醇很容易解吸，未观察到杂环胺的残留。从杂环胺面积计数与作为内标的 4,7,8-TriMeIQx 的面积计数比率获得的校准曲线在 5 至 200 ng mL(-1) 范围内呈线性，相关系数高于 0.9976 (n = 18)。检测限(S/N=3)为0.2-3.1 ng·mL(-1)。该方法已成功应用于食品样品的分析。
In-tube solid-phase microextraction (in-tube SPME) coupled with liquid chromatography/electrospray ionization mass spectrometry (LC/ESI-MS) was developed for the analysis of mutagenic heterocyclic amines. LC/MS analyses of heterocyclic amines were initially performed by liquid injection onto a LC column. All heterocyclic amines tested in this study gave very simple ESI mass spectra and strong signals corresponding to [M + H](+) were observed for all heterocyclic amines except for Glu-P-1 and Glu-P-2 ([M + NH(4) - H(2)O](+) ions were observed from these amines). All heterocyclic amines were well separated with a Supelcosil LC-CN column except for A alpha C and Glu-P-2 which consistently co-eluted. In order to optimize the extraction of heterocyclic amines, several in-tube SPME parameters were examined using five representative compounds. The optimum extraction conditions were as follows: 10 aspirate/dispense steps of 30 mu L of sample in 100 mM Tris-HCl (pH 8.5) at the flow rate of 100 mu L min(-1) with Omegawax 250 capillary column. The heterocyclic amines extracted by the capillary column were easily desorbed by aspiration of 30 mu L of methanol prior to injection, and carryover of heterocyclic amine was not observed. The calibration curves obtained from the ratios of heterosyclic amine area counts against that of 4,7,8-TriMeIQx as an internal standard were linear in the range of 5 to 200 ng mL(-1), with correlation coefficients above 0.9976 (n = 18). The detection limits (S/N = 3)were 0.2-3.1 ng mL(-1). This method was successfully applied to the analysis of food samples.