EDTA络合提取-GFAAS法测定藿香正气丸中的铝离子残留

Determination of residual aluminium Ion in Huoxiang Zhengqi pellets by GFAAS with EDTA complexation extraction

建立了免消化处理的乙二胺四乙酸二钠（EDTA）络合提取,结合GFAAS法测定藿香正气丸中的铝离子残留。对样品前处理方法进行了系统研究,采用EDTA对样品中铝离子进行络合提取,对萃取溶剂pH,浓度,体积,微波萃取温度,时间,石墨炉升温程序进行了优化考察,并与微波消解法测定结果比较。结果表明,0.1 g样品加入0.05 mol·L^-1EDTA溶液20 mL（pH 3.5）,以150℃微波萃取10 min,进一步在257.4 nm检测波长及优化的石墨炉升温程序下进行GFAAS的测定。方法的检测限为2.37μg·L^-1,定量限为7.89μg·L^-1,精密度RSD小于2.3%,平均回收率为96.9%-101%。该法简单、快速、准确,可用于快速检测中成药中的铝离子残留。

To establish an EDTA complexation extraction pretreatment combining with GFAAS method for the determination of residual aluminium ion in Huoxiang zbengqi pellets without digestive treatment, systematical investigation was made on sample preparation, and EDTA was used for the complexation extraction of residual aluminium ion in samples. The pH, concentration and volume of extraction solution, the temperature and time of microwave extraction, and graphite furnace temperature program were investigated. The results were compared with the microwave digestion. It was showed that, 0. 1 g of sample weight was added in 20 mL 0. 05 mol· L^-1 EDTA solution （pH 3. 5）, followed by heating at 150 ℃ for 10 min in the microwave extraction device. The determination of GFAAS was performed at optimized detection wavelength （257.4 nm） as well as graphite furnace temperature program, the detection limits and quantification limits were 2. 37 μg·L^-1 and 7. 89μg·L^-1 , respectively. The precision （RSD） was less than 2. 3%. The average re- covery was 96. 9% -101%. The present method is easy, rapid and accurate for the determination of residual aluminium ion in Huoxiang zhengqi pellets.