da Silveira Géssica Domingos, Faccin Henrique, Claussen Luis, Goularte Rayane Bueno, Do Nascimento Paulo C, Bohrer Denise, Cravo Margareth, Leite Leni F M, de Carvalho Leandro Machado
Department of Chemistry, Federal University of Santa Maria (UFSM), Santa Maria-RS, Brazil; Graduate Program in Chemistry, Federal University of Santa Maria (UFSM), Santa Maria-RS, Brazil.
Centro de Pesquisa e Desenvolvimento "Leopoldo Américo Miguez de Mello (CENPES), PETROBRAS, Rio de Janeiro, RJ, Brazil.
J Chromatogr A. 2016 Jul 29;1457:29-40. doi: 10.1016/j.chroma.2016.06.003. Epub 2016 Jun 3.
We present a sensitive liquid chromatography-atmospheric pressure photoionization tandem mass spectrometric (UHPLC-APPI-MS/MS) method for the determination of selected organosulfur compounds in Brazilian asphalt cements. It was possible to detect 14 organosulfur compounds of different classes where sulfoxides and sulfones presented higher sensibility in ionization than thiophenes and aromatic sulfides. A dopant-assisted APPI method was also tested, however, when chromatographic flow rate was optimized a decrease in signal was observed for all compounds. PAHs were tested and ruled out as possible interfering compounds and the matrix effect of asphalt cements was within an acceptable range for the quantification of organosulfur compounds. The proposed method was found to have satisfactory linearity and accuracy with recoveries between 83.85 and 110.28% for thianaphthene and 3-methylbenzothiophene, respectively. Therefore, the method allowed the characterization of organosulfur compounds in Brazilian asphalt cements and demonstrated changes in the amount quantified in asphaltenic and maltenic fractions after the RTFOT+SUNTEST aging process.
我们提出了一种灵敏的超高效液相色谱-大气压光电离串联质谱法（UHPLC-APPI-MS/MS），用于测定巴西沥青水泥中的特定有机硫化合物。可以检测到14种不同类别的有机硫化合物，其中亚砜和砜在电离方面比噻吩和芳族硫化物具有更高的灵敏度。还测试了掺杂剂辅助的APPI方法，然而，当优化色谱流速时，观察到所有化合物的信号均下降。对多环芳烃进行了测试，并排除了其作为可能干扰化合物的可能性，并且沥青水泥的基质效应在有机硫化合物定量的可接受范围内。结果发现，所提出的方法具有令人满意的线性和准确性，硫茚和3-甲基苯并噻吩的回收率分别在83.85%至110.28%之间。因此，该方法能够对巴西沥青水泥中的有机硫化合物进行表征，并证明了在RTFOT+SUNTEST老化过程后，沥青质和软沥青质馏分中定量的有机硫化合物含量发生了变化。
