首页> 外文期刊>Journal of liquid chromatography and related technologies >DETERMINATION OF NATAMYCIN CONTENT IN CHEESE USING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY
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DETERMINATION OF NATAMYCIN CONTENT IN CHEESE USING ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY-MASS SPECTROMETRY

机译:高效液相色谱-质谱法测定奶酪中的纳他霉素含量

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摘要

Nalamycin is a fungistatic antibiotic that is used therapeutically only for a surface treatment and does not cause resistance of yeasts and fungi. It has a broad spectrum of activity for most yeasts and fungi that come into consideration in food. A methods based on the use of ultra-performance liquid chromatography tandem mass spectrometry (UPLC/ MS/ MS) and lime of flight mass spectrometry (UPLC/ TOF MS) interfaced with eleclrospray were devised for determination of nalamycin content in cheese samples. Sample preparation included, extraction offal and protein removal by congelation. In case of loiv concentrations of nalamycin, extract was concentrated by SPE. UPLC was performed on an Acquily UPLC BEH C18 (100mm x 2.1mm). UPLC/TOF data were acquired in TOF MS full scan mode. UPLC/MS/MS data acquisition was achieved using multiple reaction monitoring (MRM). The elaborated methods for determination of nalamycin in cheese were validated. Detection limits vary depending on the mass spectrometer. For UPLC/ TOF detection limit is 50 ng- kg"', for the the triple quadrupole 5 mugkg"1. The relative standard deviation (RSD) of the method was for the UPLC/TOF, 3%, and for UPLC/MS/MS, 5.3%. The described methods meet all the criteria of Decision 2002/657/EC and are easy to use in routine analyses.
机译:那拉霉素是一种抑菌抗生素,仅在治疗上用于表面处理,不会引起酵母和真菌的耐药性。它对食品中考虑的大多数酵母和真菌具有广泛的活性。设计了一种基于超高效液相色谱串联质谱法(UPLC / MS / MS)和飞行石灰法(UPLC / TOF MS)结合电子喷雾的方法,用于测定奶酪样品中的那拉霉素含量。样品制备包括提取内脏和通过凝胶去除蛋白质。在低浓度的那拉霉素的情况下,通过SPE浓缩提取物。在Acquily UPLC BEH C18(100mm x 2.1mm)上执行UPLC。 UPLC / TOF数据是在TOF MS全扫描模式下获取的。使用多反应监测(MRM)实现了UPLC / MS / MS数据采集。验证了测定奶酪中那拉霉素的详尽方法。检测限因质谱仪而异。对于UPLC / TOF,检出限为50 ng- kg“',对于三重四极杆5 mugkg”'。该方法的相对标准偏差(RSD)对于UPLC / TOF为3%,对于UPLC / MS / MS为5.3%。所描述的方法符合Decision 2002/657 / EC的所有标准,并且易于在常规分析中使用。

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