Derivatization in trace organic analysis: use of an all-glass conical reaction vial.
Derivatization in trace organic analysis: use of an all-glass conical reaction vial.
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痕量有机分析中的衍生化：使用全玻璃锥形反应瓶。
DOI：
10.1021/ac00046a041
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发表时间：
1992
影响因子：
7.4
通讯作者：
Giese,RW
中科院分区：
文献类型：
--
作者：
Abdel-Baky,S;Allam,K;Giese,RW
正如我们已经报道的，*1·2我们正在开发一种分析二醇环氧化物-多芳烃(DE-PAH)DNA加合物的方法，其中分离的加合物在用气相色谱-电子捕获负离子质谱仪(GC-ECNI-MS)检测之前经过三个化学步骤。这三个步骤如下：(1)酸解以四氢吡喃形式从DNA中释放出DE-PAH，(2)该四氢酚与过氧化钾氧化成相应的二羧基-多环芳烃，以及(3)后者与五氟苄基溴化物的酯化。在逐步应用该方法的步骤2和步骤3以降低真正的四氢吡喃(即苯并[a]芘-7，8，9，10-四氢四氢酚)的量的过程中，我们在100-PG水平上遇到了严重的损失和干扰。我们在此报告，这个问题是由于用于此目的的商用瓶子中存在微小的、顽固的棕色/黑色斑点，以及聚四氟乙烯衬里/塑料盖的存在。采用内部制造的全玻璃锥形反应瓶获得了可重复性的结果。
As we have reported,* 1· 2 we are developing an analytical procedure fordiol epoxide-polyaromatic hydrocarbon (DE-PAH) DNA adducts in which the isolated adducts are subjected to a sequence of three chemical steps prior to detection by gas chromatography-electron capture negative ion mass spectrometry (GC-ECNI-MS). The three steps are as follows:(1) acid hydrolysis to release the DE-PAH as a tetrol from the DNA,(2) oxidation of this tetrol with potassium superoxide to a corresponding dicarboxy-PAH, and (3) esterification of the latter compound with pentafluorobenzyl bromide.During the course of progressively applying steps 2 and 3 of the method to lower amounts of an authentic tetrol (namely benzo [a] pyrene-7, 8, 9, 10-tetrahydrotetrol), we encountered severe irreproducibility at the 100-pg level in terms of both losses and interferences. Here we report that this problem was due to microscopic, recalcitrant brown/black specks in the commercial vials employed for this purpose and the presence of PTFE liner/plastic caps. Reproducible results were achieved by employing an all-glass conical reaction vial fabricated in-house.