Komárek J, Cervenka R, Růzicka T, Kubán V
Department of Analytical Chemistry, Masaryk University, Kotlárská 2, CZ-611 37 Brno, Czech Republic.
J Pharm Biomed Anal. 2007 Nov 5;45(3):504-9. doi: 10.1016/j.jpba.2007.08.017. Epub 2007 Aug 21.
Conditions of a continuous flow extraction (CFE) of aluminium acetylacetonate in acetylacetone and aluminium 8-hydroxyquinolinate into methylisobutylketone (lengths of reaction and extraction coils, flow rates of aqueous and organic phases and their flow rate ratio, pH of aqueous phase, lengths of coils for transport of aqueous and organic phases and effect of salts) were studied. The analytical signal of the aluminium chelates present in the organic phase was measured at 309.3 nm using atomic absorption spectrometry with electrothermal atomization (ET-AAS) at the flow rate ratio F aq/F org=3 for aqueous and organic phases. The five points calibration curves were linear (R2 0.9973 and 0.9987) up to 21 microgl(-1) Al with the limits of detection of 0.3 microgl(-1) and the recovery 100+/-2% and precision of 3% at 2-10-fold dilution of the dialysis concentrates. The acetylacetonate method was applied to the determination of aluminium in real dialysis concentrates. Aluminium in concentrations 5-6 microgl(-1) (R.S.D.s 5-10% in real samples) were found and the results were in the very good agreement with those obtained by an ET-AAS using preconcentration of Al(III) on a Spheron-Salicyl chelating sorbent (absolute and relative differences were under 0.4 microgl(-1) and 8.2%, respectively).
研究了乙酰丙酮铝在乙酰丙酮中以及8-羟基喹啉铝在甲基异丁基酮中的连续流动萃取（CFE）条件（反应和萃取盘管长度、水相和有机相流速及其流速比、水相pH值、水相和有机相传输盘管长度以及盐的影响）。使用电热原子化原子吸收光谱法（ET-AAS）在水相和有机相流速比Faq/Forg = 3的条件下，于309.3 nm处测量有机相中铝螯合物的分析信号。五点校准曲线在铝浓度高达21 μg l-1时呈线性（R2分别为0.9973和0.9987），检测限为0.3 μg l-1，透析浓缩物在2 - 10倍稀释时回收率为100±2%，精密度为3%。乙酰丙酮法用于实际透析浓缩物中铝的测定。发现铝浓度为5 - 6 μg l-1（实际样品中相对标准偏差为5 - 10%），结果与使用Spheron - 水杨基螯合吸附剂预富集Al(III)的ET-AAS法所得结果非常吻合（绝对差异和相对差异分别低于0.4 μg l-1和8.2%）。
