高级检索

    大体积进样-阀切换-离子色谱法测定食用菌中高氯酸根、氯酸根、溴离子和溴酸根的含量

    Determination of Perchlorate, Chlorate, Bromide Ion and Bromate in Edible Fungi by Ion Chromatography with Large Volume Injection and Valve Switching

    • 摘要: 为避免食用菌中高含量氯离子对高氯酸根、氯酸根、溴离子和溴酸根测定的干扰,降低检出限,提出了题示研究。取匀浆好的新鲜食用菌样品10.0 g置于50.0 mL离心管中,加入40.0 mL水,振荡30 min,用水定容至50.0 mL,离心5 min。上清液过0.22 µm水相滤膜,滤液采用离子色谱法分析。以Dionex IonPac AS19色谱柱作分析柱,氢氧化钾溶液梯度淋洗,设置排废模式0~5.8 min、进样模式5.9~25.0 min的阀切换时间,电导检测器检测上述4种阴离子。结果表明,高氯酸根、氯酸根、溴酸根的质量浓度在10.0~1 000.0 μg·L−1内,溴离子在1.0~1 000.0 μg·L−1内和对应的响应强度呈线性关系,检出限(3S/N)为5.0~50.0 μg·kg−1。按照标准加入法进行回收试验,回收率为80.1%~96.5%,测定值的相对标准偏差(n=6)为2.1%~4.2%。方法用于分析30份食用菌样品,高氯酸根检出量为50.0~3 213.6 μg·kg−1,溴离子检出量为214.1~1 236.5 μg·kg−1,氯酸根和溴酸根均未检出。

       

      Abstract: In order to avoid the interference of high contents of chloride ions in edible fungi on the determination of perchlorate, chlorate, bromide ion, and bromate, and reduce the detection limits, the study mentioned by title was proposed. A fresh homogenized edible fungi sample (10.0 g) was taken and placed in a 50.0 mL-centrifuge tube, and 40.0 mL of water was added. The mixture was oscillated for 30 min, made its volume up to 50.0 mL with water, and centrifuged for 5 min. The supernatant was filtered through a 0.22 µm water phase filter membrane, and the filtrate was analyzed by the ion chromatography. Using Dionex IonPac AS19 chromatographic column as the analytical column, potassium hydroxide solution was used for gradient elution. The valve switching time was set at 0-5.8 min in waste discharge mode and 5.9-25.0 min in injection mode, and the above 4 anions in the filtrate was detected by conductivity detector. As shown by the results, linear relationships between values of the mass concentration and the response intensity were kept in the range of 10.0-1 000.0 μg · L−1 for perchlorate, chlorate and bromate, and 1.0-1 000.0 μg · L−1 for bromide ion, with detection limits (3S/N) in the range of 5.0-50.0 μg · kg−1. Test for recovery was made by the standard addition method, giving recoveries in the range of 80.1%-96.5%, with RSDs (n=6) of the determined values in the range of 2.1%-4.2%. This method was used for analysis of 30 edible fungi samples, the detection amounts of perchlorate were in the range of 50.0-3 213.6 μg · kg−1, the detection amounts of bromide ion were in the range of 214.1-1 236.5 μg · kg−1, and chlorate and bromate were not detected.

       

    /

    返回文章
    返回