土霉素
检出限
色谱法
洗脱
毛细管电泳
化学
固相微萃取
最大残留限量
离子强度
萃取(化学)
纤维
吸附
水溶液
农药残留
气相色谱-质谱法
杀虫剂
质谱法
有机化学
物理化学
抗生素
生物
生物化学
农学
作者
T. Alexandra Ferreira,Juan Francisco Flores-Aguilar,Eva M. Santos,José A. Rodríguez,Israel S. Ibarra
出处
期刊:Molecules
[MDPI AG]
日期:2019-01-24
卷期号:24 (3): 430-430
被引量:21
标识
DOI:10.3390/molecules24030430
摘要
In this work, a procedure using solid phase microextraction in combination with capillary electrophoresis was developed for the determination of oxytetracycline in milk samples. The method involves the synthesis of poly(1-allyl-3-methyl imidazolium) chloride film on a stainless-steel bar via electropolymerization and its use as an adsorbent for oxytetracycline (OT) by an ionic exchange mechanism. The coated fiber is then immersed in milk samples for retention of oxytetracycline residues, followed by elution, drying, and reconstitution before analysis with capillary electrophoresis. The proposed method achieves a limit of detection of 70 µg L–1 with adequate precision and uncertainty, making this methodology appropriate for the determination of OT in milk samples. The method was applied to the pre-concentration and quantification of oxytetracycline in ten commercial milk samples. Two tested samples were positive for the presence of oxytetracycline but the concentration was below the maximum residue limit according to the international normative standard. The proposed methodology was evaluated according to the Eco-Scale approach, and the total score of 51 indicated that the methodology proposed is both green and acceptable despite the multi-stage character. SPME-CE methodology allows us to perform the sample pre-treatment and determination of OT in an effective and greener way, decreasing the number of steps during the analysis and the generation of waste.
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