首页> 中文期刊>分析测试学报 >高效毛细管电泳法同时分离检测土壤中三嗪类与磺胺类抗球虫药物的研究

高效毛细管电泳法同时分离检测土壤中三嗪类与磺胺类抗球虫药物的研究

     

摘要

A high performance capillary electrophoresis method for the simultaneous separatinon and determination of four anticoccidial drugs (e. g. sulfanilamide, sulfaclozine, sulfaquinoxaline, diclazur-il) in soil was developed by using 0. 1 mol/L NaOH and THF(3:2) as extraction solution. The effects of some important factors such as pH value, composition and concentration of running buffer, separation voltage and separation temperature, were investigated, and the orthogonal test factors were optimized. The optimal conditions were as follows; the running buffer; 50 mmol/L borax -200 mmol/ L boric acid (pH 9.0), separation voltage; 23 kV, separation temperature: 25 X., UV detection wavelength; 220 nm and 254 nm. Under the optimal chromatographic conditions, the four anticoccidi al drugs can be well separated within 7.0 min. The calibration curves of four anticoccidial drugs were linear in the range of 1.56 -50 mg/L with correlation coefficients (r2) of 0. 994 7-0. 999 9. The average recoveries of four anticoccidial drugs in soil sample at three spiked concentration levels of 2. 0, 5.0, 10 mg/kg ranged from 77% to 90%, with relative standard deviations (RSDs, n= 6) of 6.3% -8.1% . The method was simple, rapid and low-cost, and was successfully applied in the determination of four anticoccidial drugs in the soil of poultry farms.%以体积比为3:2的0.1 mol/L NaOH和THF混合液作为提取液,建立了同时分离检测土壤中两类抗球虫药物(磺胺、磺胺氯吡嗪、磺胺喹(噁)啉、地克珠利)的高效毛细管电泳(HPCE)方法.考察了HPCE中缓冲液类型、离子浓度和pH值、分离电压、分离温度等因素,利用正交实验进行条件优化,得出了最佳实验条件:缓冲体系为50 mmol/L硼砂-200 mmol/L硼酸(pH 9.0),分离电压23 kV,分离温度25℃,紫外检测波长分别为220 nm和254 nm.在此最佳分离条件下,上述4种抗球虫药物在7.5 min内实现快速分离.4种药物在1.56~ 50 mg/L范围内呈良好线性,相关系数(r2)为0.9947~0.9999.在2.0、5.0、10.0 mg/kg的加标水平下,4种药物的回收率为77% ~90%,相对标准偏差(RSDs,n=6)为6.3%~8.1%.该方法简便、快速、成本低,成功应用于畜禽养殖场土壤中4种常用抗球虫药物的快速检测.

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