کد مقاله | کد نشریه | سال انتشار | مقاله انگلیسی | نسخه تمام متن |
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1210488 | 965374 | 2009 | 5 صفحه PDF | دانلود رایگان |
![عکس صفحه اول مقاله: In-house validation of liquid chromatography tandem mass spectrometry for determination of semicarbazide in eggs and stability of analyte in matrix In-house validation of liquid chromatography tandem mass spectrometry for determination of semicarbazide in eggs and stability of analyte in matrix](/preview/png/1210488.png)
An improved LC-MS/MS method for the determination of semicarbazide in whole egg is described. Waters OASIS-MCX cation exchange purification cartridges increased the sensitivity for analysis by LC-MS/MS. The validation study was carried out according to criteria and requirements of Commission Decision 2002/657/EC for confirmatory analysis and provided the data as follows: The correlation coefficient for the matrix calibration curve, in the range of 0–5 μg kg−1, was r = 0.9968. The detection capability and decision limit, measured according to ISO11843-2, were CCα = 0.20 μg kg−1 and CCβ = 0.25 μg kg−1. Repeatability (CVSr) and within-laboratory reproducibility (CVSwr) determined for the concentration levels of 0.2, 0.5 and 1.0 μg kg−1 SEM ranged from 11.9 to 5.7% and 11.8 to 6.3%, respectively. The validated method was applied to investigate SEM stability in incurred materials (egg homogenates) during long-term storage at −20 °C and 4 °C. The study proved by a two-sampling test that SEM at levels of 17. 7, 1.2, 10.6 and 0.47 μg kg−1 was stable for up to 12 months.
Journal: Journal of Chromatography A - Volume 1216, Issue 46, 13 November 2009, Pages 8187–8191