鸡排泄物中洛克沙胂与多价态As的分离与测定方法研究

Studies on the Separation and Determination of Roxarsone and Multi Valence As in the Excreta of Chicken

对鸡排泄物中洛克沙胂、总As及无机As(Ⅲ)和As(Ⅴ)的分离与测定进行了研究.采用磷酸氢二钾-甲醇混合液提取和载入固相萃取小柱净化,对洛克沙胂进行HPLC法分析,回收率≥74.4%,最低检测限为0.1μg/g.经微波消解处理后采用AFS法检测排泄物中总As含量,检出限为0.08μg/L,回收率≥94.7%.经磷酸二氢钾溶液振荡提取过滤后,依次经阳离子和阴离子交换树脂静态吸附与动态分离,采用AFS法分别测定As(Ⅲ)、As(Ⅴ)含量,检出限分别为0.084和0.210μg/L,回收率分别为87.8%～113.0%和81.1%～127.3%.

The methods based on HPLC and AFS for the separation and determination of roxarsone, total arsenic,As（ Ⅲ ）and As（ Ⅴ ）in the excreta of chicken were established. The excreta were extracted with K2 HPQ-CH3 OH, cleaned-up by Straxa-X-AW SPE column and quantified with HPLC system. The recovery was all over 74.4%, and LOD was 0. 1 μg/g. A microwave digestion-atomic fluorescence spectrometry （AFS） method for determination of total arsenic was applied. The excreta were digested in a closed vessel device and determinated by AFS. The LOD was 0. 08 μg/L and the recovery was all over 94. 7%. An ion exchange resin coupled with AFS method was also developed for isolating and determinating As （Ⅲ） and As（ Ⅴ ）. The excreta were extracted with KH2PO4 ,separated by cation and anion exchange resin Ⅲ ） and and de- termined by AFS. The LODs of As（ Ⅲ ）and As（ Ⅴ）were 0. 084 and 0. 210 μg/L respectively. The recoveries of 87.8% - 113.0% for As（ Ⅲ ）and 81.1% - 127.3% for As（ Ⅴ ） were obtained.