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    磁性竹炭为吸附剂的分散基质固相萃取分离-高效液相色谱法测定水中双酚S的含量

    HPLC Determination of Bisphenol S in Water with Separation by Solid Phase Extraction in Matrix Dispersion Using Magnetic Bamboo Charcoal as Adsorbent

    • 摘要: 用稀硝酸将水样(100.0 mL)的pH调整至4,加入2.5 g氯化钠和自制的磁性竹炭30 mg,旋涡振荡8 min,使双酚S吸附于磁性竹炭,丢弃水相,加入甲醇0.5 mL旋涡振荡2 min,使双酚S解吸并溶于甲醇中。所得溶液以Spherigel C18色谱柱为固定相,以乙腈(55+45)溶液为流动相进行高效液相色谱分离和紫外检测。双酚S的质量浓度在0.1~20 μg·L-1内与其峰面积呈线性关系,检出限(3S/N)为0.05 μg·L-1。按上述方法测定1.0 μg·L-1双酚S标准溶液7次,其测定值的相对标准偏差为5.6%。按标准加入法进行回收试验2次,回收率分别为88.7%,90.6%。

       

      Abstract: The water sample (100.0 mL) was adjusted to pH 4 with dilute nitric acid. 2.5 g of NaCl and 30 mg of self-prepared magnetic bamboo charcoal (MBC) were added into the sample solution. The above mixture was swirled for 8 min to have bisphenol S adsorbed on MBC. The aqueous phase was discarded. Methanol (0.5 mL) was added to the solid phase and the mixture was swirled for 2 min to desorb bisphenol S from MBC into methanol. The methanol solution was separated by HPLC using Spherigel C18 chromatographic column as stationary phase, and a mixture of acetonitrile and H2O (55+45) as mobile phase. UV-detection was adopted. Linear relationship between values of peak area and mass concentration of bisphenol S was found in the range of 0.1-20 μg·L-1, with detection limit (3S/N) of 0.05 μg·L-1. 1.0 μg·L-1 standard solution of bisphenol S was determined by the above method for 7 times, giving value of RSD of 5.6%. Two determination were made in testing for recovery by standard addition method, values of recovery found were 88.7% and 90.6%.

       

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