Determination of Benzidine in Soil by High Performance Liquid Chromatography with Ultrasonic Extraction
摘 要
取干燥的土壤样品5.00 g,用含有1%(体积分数)氨水和50 mg·L-1硫代硫酸钠(防止联苯胺的氧化)的甲醇溶液(作为提取剂)10 mL超声提取30 min,加冰保持温度低于10℃,静置10 min。取上清液2.0 mL,经0.22 μm聚四氟乙烯针式过滤器过滤后,以ZORBAX C18反相色谱柱为固定相,体积比25:75的乙腈-0.01 mol·L-1乙酸铵溶液的混合液为流动相,直接采用附荧光检测器的高效液相色谱法测定其中联苯胺的含量。结果表明,联苯胺的质量浓度在0.50~50.0 μg·L-1内与对应的峰面积呈线性关系,检出限为0.20 μg·kg-1。按标准加入法对空白土壤样品进行回收试验,回收率为75.9%~99.1%,测定值的相对标准偏差(n=6)均小于4.0%。
Abstract
5.00 g of dry soil sample was taken and extracted ultrasonically for 30 min in 10 mL of methanol solution (as extractant) containing 1% (volume fraction) ammonia and 50 mg·L-1 sodium thiosulfate (to prevent the oxidation of benzidine). Ice was added to keep the temperature below 10℃, and the mixture was settled for 10 min. 2.0 mL of the supernatant was taken and passed through 0.22 μm polytetrafluoroethylene needle filter. Benzidine in the filtrate was directly determined by high performance liquid chromatography with fluorescence detector, with ZORBAX C18 reversed-phase chromatographic column as the stationary phase and a mixture of acetonitrile and 0.01 mol·L-1 ammonium acetate solution at a volume ratio of 25:75 as the mobile phase. As shown by the results, linear relationship between values of peak area and mass concentration of benzidine was found in the range of 0.50-50.0 μg·L-1, with detection limit of 0.20 μg·kg-1. Test for recovery was made on blank soil sample by standard addition method, giving results in the range of 75.9%-99.1%, with RSDs (n=6) of the determined values less than 4.0%.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202203014
所属栏目 工作简报
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收稿日期 2021/2/23
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备注那晶晶,工程师,硕士,研究方向为环境分析测试,550983032@qq.com
引用该论文: NA Jingjing,DAI Xuanli,XU Xuejuan,XIA Fei. Determination of Benzidine in Soil by High Performance Liquid Chromatography with Ultrasonic Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(3): 329~332
那晶晶,戴玄吏,徐雪娟,夏飞. 超声提取-高效液相色谱法测定土壤中联苯胺的含量[J]. 理化检验-化学分册, 2022, 58(3): 329~332
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参考文献
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【2】陶云锋,陆亮,崔静,等.ASE-GPC-GC/MS同时测定土壤中16种苯胺类物质[J].环境科学与技术, 2019,42(2):151-156.
【3】刘德辉,代飞飞,聂丹丹.气相色谱-质谱法测定水中19种苯胺类化合物[J].中国城乡企业卫生, 2016,31(5):66-69.
【4】张秀蓝,郭婧,任立军,等.HPLC-FLD测定水中联苯胺的方法研究[J].中国环境监测, 2017,33(3):160-164.
【5】张明,唐访良,徐建芬,等.超高效液相色谱-串联质谱法快速测定地表水中联苯胺、苦味酸、甲萘威、阿特拉津和溴氰菊酯[J].色谱, 2018,36(9):866-872.
【6】宋环宇,沈振华.三重四极杆液相色谱/质谱法直接测定水中联苯胺[J].环境与发展, 2018,30(5):122-122.
【7】杨静.高效液相色谱-串联三重四极杆质谱法测定土壤中苦味酸和联苯胺[J].中国环境监测, 2020,36(4):145-153.
【8】生态环境部办公厅.关于征求《土壤和沉积物钴的测定火焰原子吸收分光光度法》等六项国家环境保护标准意见的函.环办标征函(2018)68号[EB/OL]. (2018-12-13)[2019-01-05]. http://www.mee.gov.cn/xxgk2018/xxgk/xxgk06/201812/t20181211_684235.html.
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