Singh Vandana, Gupta Manju, Jain Archana, Verma Krishna K
Department of Chemistry, Rani Durgavati University, Jabalpur, Madhya Pradesh 482001, India.
J Chromatogr A. 2003 Aug 29;1010(2):243-53. doi: 10.1016/s0021-9673(03)01123-3.
Derivatization of aromatic primary amines to N-allyl-N'-arylthioureas by reaction with allyl isothiocyanate and GC-MS of the derivatives, when pyrolysis to aryl isothiocyanates occurs in the heated injector, has been used to determine aromatic amines in the range 0.5-50 microg l(-1) with a correlation coefficient, r, in the range 0.9902-0.9992. The limit of detection ranged 8 to 30 ng l(-1) when 60 ml of sample were preconcentrated, after derivatization, on a styrene-divinylbenzene copolymer sorbent. The pyrolytic cleavage of sym- and unsym-diaryl or alkyl-/arylthioureas has been rationalized. The chromatography of isothiocyanates is much superior to that of aryl amines and the specific mass fragmentation permits positive identification of amines. The method has been applied to spiked drinking water, groundwater and river water samples, when the recovery ranged from 84 to 109% with RSD of 5-9%, and to detect aromatic amines formed by reductive cleavage of azo dyes in effluents when the recovery of amine was in the range 81-95% with RSD 8-15%. The method is not applicable to nitroanilines.
通过与异硫氰酸烯丙酯反应将芳香伯胺衍生化为N - 烯丙基 - N'-芳基硫脲，并对衍生物进行气相色谱 - 质谱联用分析。当在加热进样器中发生热解生成芳基异硫氰酸酯时，该方法已用于测定浓度范围为0.5 - 50 μg l⁻¹的芳香胺，相关系数r在0.9902 - 0.9992之间。当60 ml样品在衍生化后在苯乙烯 - 二乙烯基苯共聚物吸附剂上进行预浓缩时，检测限范围为8至30 ng l⁻¹。对称和不对称二芳基或烷基/芳基硫脲的热解裂解已得到合理说明。异硫氰酸酯的色谱分析远优于芳基胺，且特定的质量碎片可用于胺的阳性鉴定。该方法已应用于加标饮用水、地下水和河水样品，回收率在84%至109%之间，相对标准偏差为5 - 9%；还用于检测废水中偶氮染料还原裂解形成的芳香胺，胺的回收率在81%至95%之间，相对标准偏差为8 - 15%。该方法不适用于硝基苯胺。
