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8 Linearity range and lower limit of determination
According to the sensitivity of sulfa drugs, a series of matrix 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 20L, and the peak area is used to compare the tested group in the matrix standard working solution.
Concentrations of the components are plotted, and the linear range, linear equation and linear correlation coefficient are shown in Table 2-12
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Table 2-12 Linear ranges, linear equations and correlation coefficients of 18 sulfonamides
It can be seen that under the operating conditions of this method, the 18 kinds of sulfonamides show a linear relationship in the range of 2-100ug/kg, and the minimum detection limit of the method is determined with the signal-to-noise ratio of each sulfonamide peak height greater than 5
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The limit of detection (LOD) of the 18 sulfonamides is 2.
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9 Method recovery and precision
Use royal jelly samples without sulfa drugs to perform addition recovery and precision experiments.
After adding different concentrations of standards to the samples, shake them up and leave them for 1 hour to make the standards fully absorbed by the sample, and then perform extraction and purification according to this method.
Chromatography-tandem quadrupole mass spectrometry determination, the recovery rate and precision results are shown in Table 2-13
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It can be seen from Table 2-13 that the recovery rate of this method is between 80.
Table 2-13 The recovery rate and precision experiment results of sulfa addition in royal jelly (n=10)
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10 Repeatability and reproducibility
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 2-14 Content range and repeatability and re-limiting equation
