Liquid chromatography analysis of carbonyl (2,4-dinitrophenyl)hydrazones with detection by diode array ultraviolet spectroscopy and by atmospheric pressure negative chemical ionization mass spectrometry
Liquid chromatography analysis of carbonyl (2,4-dinitrophenyl)hydrazones with detection by diode array ultraviolet spectroscopy and by atmospheric pressure negative chemical ionization mass spectrometry
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DOI：
10.1021/ac981022v
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发表时间：
1999-05-01
影响因子：
7.4
通讯作者：
Grosjean, D
中科院分区：
文献类型：
--
作者：
Grosjean, E;Green, PG;Grosjean, D
通过液相色谱法分离羰基化合物的 (2,4-二硝基苯基)腙，并通过紫外光谱（二极管阵列检测器）和大气压负化学电离质谱检测，给出了 78 种羰基化合物的结果，其中包括 18 种 1-烷醛（从甲醛到十八醛）、16 种其他饱和脂肪族羰基化合物（5 个 C-4-C-7 醛和 11 个 C-3-C-9）酮）、16 个不饱和脂肪族羰基（9 个 C-3-C-11 醛和 7 个 C-4-C-9 酮）、13 个芳香族羰基（包括羟基和/或甲氧基取代的化合物）、10 个 C-2-C-10 脂肪族二羰基、3 个脂肪族羰基酯和 2 个其他羰基，观察到异构体带有其他含氧取代基的α，β-不饱和酮和饱和羰基，例如甲氧基丙酮、2-糠醛和 3 羰基酯，对于所研究的所有羰基化合物（除其中两个之外），负 APCI 质谱中的基峰是 M - 1 离子 (NO2)(2)C6H3NN=CR1R2（对于醛，R-1 = H），其中 M 是羰基（2,4-二硝基苯基）腙衍生物的分子量。二羰基 2,4-戊二酮和琥珀二醛与 DNPH 反应主要产生其他产物。通过紫外光谱法（峰面积）和质谱法（RI - 1 离子丰度）测量的浓度非常一致。所描述的应用包括测量城市空气中浓度为十亿分之 0.015-14 的 34 C-1-C-18 羰基化合物，以及在不饱和有机化合物大气氧化的实验室研究中鉴定 ppb 浓度的羰基化合物作为反应产物。
The (2,4-dinitrophenyl)hydrazones of carbonyls are separated by liquid chromatography and detected by ultraviolet spectroscopy (diode array detector) and by atmospheric pressure negative chemical ionization mass spectrometry, Results are presented for 78 carbonyls including 18 1-alkanals (from formaldehyde to octadecanal), 16 other saturated aliphatic carbonyls (5 C-4-C-7 aldehydes and 11 C-3-C-9 ketones), 16 unsaturated aliphatic carbonyls (9 C-3-C-11 aldehydes and 7 C-4-C-9 ketones), 13 aromatic carbonyls (including hydroxy- and/or methoxy-substituted compounds), 10 C-2-C-10 aliphatic dicarbonyls, 3 aliphatic carbonyl esters, and 2 other carbonyls, Isomers were observed for alpha,beta-unsaturated ketones and saturated carbonyls that bear other oxygen-containing substituents, e,g. methoxyacetone, 2-furaldehyde, and the 3 carbonyl esters, For ail but two of the carbonyls studied, the base peak in the negative APCI mass spectrum was the M - 1 ion (NO2)(2)C6H3NN=CR1R2 (R-1 = H for aldehydes), where M is the molecular mass of the carbonyl (2,4-dinitrophenyl)hydrazone derivative. The dicarbonyls 2,4-pentanedione and succinic dialdehyde reacted with DNPH to yield predominantly other products. Concentrations measured by ultraviolet spectroscopy (peak area) and by mass spectrometry (abundance of RI - 1 ion) were in good agreement. Applications described include the measurement of 34 C-1-C-18 carbonyls at levels of 0.015-14 parts per billion (ppb) in urban air and the identification of carbonyls at ppb concentrations as reaction products in laboratory studies of the atmospheric oxidation of unsaturated organic compounds.