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8 Linearity range and lower limit of determination
According to the sensitivity of sulfa drugs, a series of mass-based standard working solutions are prepared with sample blank solution, and the determination is carried out under selected chromatographic conditions and mass spectrometry conditions.
The sample volume is 40μL, and the peak area is used to measure the matrix standard working solution.
The concentration of the components is plotted, and the linear range, linear equation and linear correlation coefficient are shown in Table 2-16
.
Table 2-16 Linear ranges, linear equations and correlation coefficients of 16 sulfonamides
It can be seen that under the operating conditions of this method, sulfamethizole 1.
0-25.
0μg/kg, sulfacetamide , sulfadiazine, sulfachloropyridazine , sulfamethoxazole, sulfamethazine, sulfapyridine , Sulfamethoxazole 2.
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2.
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9 Method recovery and precision
Use poultry tissue samples without sulfa drugs to perform addition recovery and precision experiments.
After adding different concentration standards to the samples, leave them for 1 hour to allow the standards to be fully absorbed by the sample, and then perform extraction and purification according to this method, using liquid chromatography- The recovery and precision results of tandem quadrupole mass spectrometry are shown in Table 2-17
.
It can be seen from Table 2-17 that this method has four addition levels of 2.
Table 2-17 Sulfonamide addition recovery rate and precision test results in livestock and poultry meat (n=8)
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Under repeatability test conditions, the absolute difference between the two independent test results obtained does not exceed the repeatability limit (r).
If the difference exceeds the repeatability limit (r), the test results should be discarded and the two single tests should be completed again.
Determination
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Under the reproducibility test conditions, the absolute difference between the two independent test results obtained does not exceed the reproducibility limit (R)
Table 2-18 Content range and repeatability and reproducibility equation
Related links: Determination of 16 sulfonamide residues in livestock and poultry meat by liquid chromatography-tandem mass spectrometry (2)