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Determination of salicylic acid in feed using LC-MS/MS

机译:使用LC-MS / MS测定饲料中的水杨酸

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Introduction: Salicylic acid is a derivative of benzoic acid and occurs in nature. The main target of this study was to develop the liquid chromatography coupled with tandem mass spectrometry technique as a method for determination of salicylic acid in feed materials and compound feed. Material and Methods: Salicylic acid was extracted from feed with 0.1% hydrochloric acid in methanol. Separation was achieved in 8 min in a gradient elution using 0.1% formic acid and acetonitrile. The analyte was detected using negative electrospray tandem mass spectrometry. The procedure was validated to the specifications of the European Commission Decision No. 2002/657/EC. Results: The validation results showed the repeatability of the method, which was evaluated at three levels (0.25, 0.5, and 1.0 mg/kg). Calibration curves for the working ranges were linear (R-2 0.9911 to 0.9936), and recoveries ranged from 98.3% to 101%. The LOD and LOQ for compound feed were 0.02 and 0.05 mg/kg, respectively. Salicylic acid was found mostly in corn, and its concentrations differed depending on whether it was young or fully grown (5.30-12.8 mg/kg and 0.13-1.01 mg/kg, respectively). Conclusions: A sensitive and reliable method for the determination of salicylic acid in feed and compound feed using LC-MS/MS was developed.
机译:介绍:水杨酸是苯甲酸的衍生物,并且在自然界中发生。该研究的主要目标是开发与串联质谱技术相结合的液相色谱,作为饲料材料中水杨酸和化合物进料中的水杨酸的方法。材料和方法:在甲醇中用0.1%盐酸萃取水杨酸。在使用0.1%甲酸和乙腈的梯度洗脱中,在8分钟内实现分离。使用负电喷雾串联质谱法检测分析物。该程序验证到欧洲委员会第2002/657号/ EC的规格。结果:验证结果表明该方法的可重复性,其在三个水平下评估(0.25,0.5和1.0mg / kg)。工作范围的校准曲线是线性的(R-2 0.9911至0.9936),回收率范围为98.3%至101%。复合饲料的LOD和LOQ分别为0.02和0.05mg / kg。在玉米中发现水杨酸,其浓度取决于它是否杨或完全生长(分别为5.30-12.8mg / kg和0.13-1.01 mg / kg)。结论:利用LC-MS / MS的饲料和化合物进料中测定水杨酸测定的敏感性和可靠方法。

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