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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Analysis of colistin A and B in fishery products by ultra performance liquid chromatography with positive electrospray ionization tandem mass spectrometry
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Analysis of colistin A and B in fishery products by ultra performance liquid chromatography with positive electrospray ionization tandem mass spectrometry

机译:高效液相色谱-电喷雾电离串联质谱法测定水产品中粘菌素A和B

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摘要

A rapid and simple method for the determination of colistin A and B in fishery products by reversed phase ultra performance liquid chromatography with positive electrospray ionization tandem spectrometry (UPLC-ESI-MS/MS) method was described. The samples were extracted with 1.0mol/L of hydrochloric acid in methanol-water and then purified on the PLS solid phase extraction columns. Then the eluate was evaporated to less than 1mL under a gentle stream of nitrogen at 40°C and formic acid-acetonitrile-water (0.2/10/90, v/v/v) was added to adjust volume to 1mL final volume. An aliquot (10μL) was injected onto the LC column for analysis with the mobile phase of 0.2% formic acid in acetonitrile and 0.2% formic acid in water at 0.20mLmin ~(-1). Multiple reaction monitoring was performed using precursor-product ion combinations. Calibration curves were linear from 200ng/mL to 2000ng/mL for colistin A and B. Mean recoveries were between 72.9% and 82.9%. The LOD was 10.0μg/kg and LOQ was 40.0μg/kg. The intra-day assay precision values for QC samples were between 2.17% and 9.00%, and inter-day values were between 2.80% and 6.97%. The method has merits of simplicity, sensitivity and rapidity, and it can be used for the determination of colistin A and B in fishery products.
机译:介绍了一种快速,简单的反相超高效液相色谱-正电喷雾电离串联质谱法(UPLC-ESI-MS / MS)测定水产品中粘菌素A和B的方法。样品用1.0mol / L盐酸的甲醇水溶液萃取,然后在PLS固相萃取柱上纯化。然后在40℃温和的氮气流下将洗脱液蒸发至小于1mL,并加入甲酸-乙腈-水(0.2 / 10/90,v / v / v)以将体积调节至1mL最终体积。将等份试样(10μL)注入LC色谱柱中,以0.20 mLmin〜(-1)的流动相在乙腈中的0.2%甲酸和在水中的0.2%甲酸的流动相进行分析。使用前体-产物离子组合进行多反应监测。大肠菌素A和B的校准曲线从200ng / mL到2000ng / mL是线性的。平均回收率在72.9%和82.9%之间。 LOD为10.0μg/ kg,LOQ为40.0μg/ kg。 QC样品的日内分析精度值在2.17%至9.00%之间,日间值在2.80%至6.97%之间。该方法具有简便,灵敏,快速的优点,可用于水产品中粘菌素A和B的测定。

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