Bellido-Martín A, Gómez-Ariza J L, Smichowsky P, Sánchez-Rodas D
Departamento de Química y Ciencia de los Materiales, Facultad de Ciencias Experimentales, Universidad de Huelva. Avda. Fuerzas Armadas s/n. 21071-Huelva, Spain.
Anal Chim Acta. 2009 Sep 7;649(2):191-5. doi: 10.1016/j.aca.2009.07.036. Epub 2009 Jul 22.
A fast extraction procedure has been developed for Sb(III) and Sb(V) oxoanions speciation in airborne particulate matter samples. Different extraction media (diammonium tartrate, hidroxilammonium clorhidrate, citric acid+ascorbic acid, phosphoric acid and citrate solutions) were tried, with assistance of an ultrasonic probe. The operation power and time of extraction were also optimized. The higher extraction recoveries were obtained with a 100 mmol L(-1) hidroxilammonium clorhidrate aqueous solution assisted by the ultrasound probe operated at 50 W during 3 min. The extracts were analyzed by HPLC-HG-AFS. The chromatographic separation of Sb(III) and Sb(V) was also optimized using diammonium tartrate and phthalic acid as mobile phases. The separation of both Sb species was performed in less than 3 min under isocratic conditions, using a 200 mmol L(-1) diammonium tartrate solution. The proposed extraction procedure and the HPLC-HG-AFS instrumental coupling have been successfully applied to airborne particulate matter samples, with high Sb content, collected in heavy traffic streets from Buenos Aires (Argentina). The results showed the presence of both Sb species at similar concentrations in the ng m(-3) level. The extraction yield was higher than 90% for all the analyzed samples.
已开发出一种快速萃取方法，用于分析空气中颗粒物样品中Sb(III)和Sb(V)含氧阴离子的形态。在超声探头辅助下，尝试了不同的萃取介质（酒石酸二铵、盐酸羟胺、柠檬酸+抗坏血酸、磷酸和柠檬酸盐溶液）。还对萃取的操作功率和时间进行了优化。使用100 mmol L(-1)盐酸羟胺水溶液，在50 W超声探头辅助下萃取3分钟，可获得较高的萃取回收率。萃取液通过HPLC-HG-AFS进行分析。还以酒石酸二铵和邻苯二甲酸作为流动相，对Sb(III)和Sb(V)的色谱分离条件进行了优化。在等度条件下，使用200 mmol L(-1)酒石酸二铵溶液，两种Sb形态在不到3分钟内即可实现分离。所提出的萃取方法和HPLC-HG-AFS仪器联用方法已成功应用于采集自阿根廷布宜诺斯艾利斯交通繁忙街道、Sb含量较高的空气中颗粒物样品。结果表明，两种Sb形态均以相似的浓度存在，处于ng m(-3)水平。所有分析样品的萃取率均高于90%。
