液体色谱法测定浓缩物、预混料和饲料中潮霉素的程序验证。
Validation of the procedure for the determination of maduramicin in concentrates, premixes, and feeds by liquid chromatography.
机构信息
Veterinary Faculty-National Veterinary Institute, University in Ljubljana, Ljubljana, Slovenia.
出版信息
Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2009 Jan;26(1):63-7. doi: 10.1080/02652030802225973.
A single laboratory validation was carried out for the determination of maduramicin in concentrates, premixes, and feed. The method comprised sample extraction of maduramicin, derivatization with dansylhydrazine and liquid chromatography with ultraviolet light detection. The limit of detection (LOD) and limit of quantification (LOQ) were 0.4 and 1.0 mg kg(-1), respectively. The repeatability expressed as the average difference between the results of duplicate measurements was 5.9% at the concentration level of 1% (concentrate), 7.1% at the concentration level of 1 g kg(-1) (premix), and 11% with the feed containing maduramicin with the nominal concentration of 5 mg kg(-1) and feed spiked at the concentration level of 1 mg kg(-1). The relative standard deviations for the within-laboratory reproducibility (RSD(W)) were 9.2%, 16%, 18%, and 17% at the concentration levels of 1%, 1 g kg(-1), 5 mg kg(-1), and 1 mg kg(-1), respectively. The measurement uncertainties were +/-0.2%, +/-0.3 g kg(-1), +/-1.9 mg kg(-1), and +/-0.3 mg kg(-1) at the same concentration levels, respectively.
本研究仅针对在浓缩物、预混料和饲料中测定土霉素的方法进行了单一实验室验证。该方法包括土霉素的样品提取、丹磺酰肼衍生化和紫外光检测的液相色谱分析。检测限（LOD）和定量限（LOQ）分别为 0.4 和 1.0 mg kg(-1)。重复性表示为在 1%（浓缩物）浓度水平下重复测量结果的平均差异，为 5.9%；在 1 g kg(-1)（预混料）浓度水平下，为 7.1%；在含有土霉素名义浓度为 5 mg kg(-1)的饲料和添加浓度为 1 mg kg(-1)的饲料中，为 11%。在浓度水平为 1%、1 g kg(-1)、5 mg kg(-1)和 1 mg kg(-1)时，实验室再现性的相对标准偏差（RSD(W)）分别为 9.2%、16%、18%和 17%。在相同浓度水平时，测量不确定度分别为+/-0.2%、+/-0.3 g kg(-1)、+/-1.9 mg kg(-1)和+/-0.3 mg kg(-1)。
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