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中国精品科技期刊2020
周小清, 冯寅洁, 汪静静. 中空纤维膜三相液相微萃取法测定猪尿及牛奶中的盐酸克伦特罗[J]. 食品工业科技, 2020, 41(1): 219-223. DOI: 10.13386/j.issn1002-0306.2020.01.035
引用本文: 周小清, 冯寅洁, 汪静静. 中空纤维膜三相液相微萃取法测定猪尿及牛奶中的盐酸克伦特罗[J]. 食品工业科技, 2020, 41(1): 219-223. DOI: 10.13386/j.issn1002-0306.2020.01.035
ZHOU Xiao-qing, FENG Yin-jie, WANG Jing-jing. Hollow Fiber Based Liquid-liquid-liquid Microextraction for the Determination of Clenbuterol in Swine Urine and Milk[J]. Science and Technology of Food Industry, 2020, 41(1): 219-223. DOI: 10.13386/j.issn1002-0306.2020.01.035
Citation: ZHOU Xiao-qing, FENG Yin-jie, WANG Jing-jing. Hollow Fiber Based Liquid-liquid-liquid Microextraction for the Determination of Clenbuterol in Swine Urine and Milk[J]. Science and Technology of Food Industry, 2020, 41(1): 219-223. DOI: 10.13386/j.issn1002-0306.2020.01.035

中空纤维膜三相液相微萃取法测定猪尿及牛奶中的盐酸克伦特罗

Hollow Fiber Based Liquid-liquid-liquid Microextraction for the Determination of Clenbuterol in Swine Urine and Milk

  • 摘要: 本文建立了中空纤维膜三相液相微萃取(hollow fiber based liquid-liquid-liquid microextraction,HF-LLLME)富集浓缩猪尿及牛奶中的痕量盐酸克仑特罗,后续采用高效液相色谱/紫外(high performance liquid chromatography with a ultraviolet detector,HPLC/UV)对其进行定量分析。对影响HF-LLLME萃取效率的因素如有机溶剂种类、选择有机萃取时间、搅拌速率以及盐效应等进行了优化,最终溶剂为甲苯,萃取时间为30 min,搅拌速率为4000 r/min,给予相中不加盐,在最优条件下,考察了该方法分析性能,结果表明:该方法在1.5~1000 μg/L内具有良好的线性(r=0.9980),方法检出限(S/N=3)、定量限(S/N=10)分别为0.5和1.5 μg/L,HF-LLLME带来的高倍浓缩效率将HPLC/UV测定克仑特罗的灵敏度提高约2个数量级。萃取过程相对标准偏差(n=7)RSD=8.8%,对猪尿和牛奶分别进行5、50、500 μg/L三个水平的加标回收实验,回收率为:猪尿87.0%~102.4%(相对标准偏差为5.1%~9.8%),牛奶80.2%~94.4%(相对标准偏差为2.7%~6.4%)。该方法富集效率高、操作简单、环保、经济、可靠,适用于定量分析尿样及牛奶等中痕量的盐酸克伦特罗。

     

    Abstract: An effective preconcentration method of hollow fiber based liquid-liquid-liquid microextraction(HF-LLLME)was proposed for the concentration of trace clenbuterol in swine urine and milk samples,and a high performance liquid chromatography with a ultraviolet detector(HPLC/UV)was used for the subsequent detection and quantification. In the process of HF-LLLME,some influence factors including the kind of organic solvent,extraction time,stirring rate and the salt effect were optimized,and toluene was finally chosen as the organic solvent,the extraction time and stirring rate were set as 30 min and 4000 r/min without salt addition in the donor phase,respectively. The analytical performance of the method was studied under the optimal conditions. Results showed a good linearity(r=0.9980)within 1.5~1000 μg/L. The limit of detection(S/N=3)was 0.5 μg/L and the limit of quantitation(S/N=10)was 1.5 μg/L. Compared with a direct injection without HF-LLLME,the high enrichment factor improve the detection sensitivity of HPLC/UV for clenbuterol by about two orders of magnitude. The recoveries at three spiked levels(5,50,500 μg/L)were 87.0%~102.4% with RSD range from 5.1% to 9.8% in swine urine and 80.2%~94.4% with RSD range from 2.7%~6.4% in milk,respectively. The method has advantages such as high enrichment efficiency,good operability,environmental protection,economic and reliability,and was successfully applied to the quantitative analysis of trace clenbuterol in swine urine and milk samples.

     

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