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5.
2.
4.
8 Linearity range and lower limit of determination
The concentrations of penicillin G, penicillin V, oxacillin , and naphthacillin were 1.
0ng/mL, 5.
0ng/mL, 10ng/mL, 50ng/mL, 100ng/mL, 200ng/mL; o-chloroxacillin , double The concentration of cloxacillin is 2.
0ng/mL, 10ng/mL, 20ng/mL, 100ng/mL, 200ng/mL, 400ng/mL honey matrix mixed standard solution, measured under the selected conditions, the injection volume is 20 Therefore, the peak area is plotted against the concentration of each component in the standard solution.
The absolute amounts of penicillin G, penicillin V, oxacillin, and naphthacillin are in the range of 0.
02 to 4 ng; o-chloropenicillin and dicloxacillin The absolute amounts of, respectively, are in a linear relationship within the range of 0.
04 ~ 8ng, which meets the quantitative requirements.
The linear equations and correction factors are shown in Table 5-31
.
Table 5-3 Linear equations and correction factors of 16 penicillins
It can be seen that under the operating conditions of this method, when the added level of 6 penicillins is in the range of 0.
5-80 μg/kg, the respective measured response values are within the linear range of the instrument
.
At the same time, the concentration of penicillin G, penicillin V, and oxacillin in the sample is 1.
5.
2.
4.
9 Method recovery and precision
Use honey samples without penicillin to perform addition recovery and precision experiments.
After adding different concentration standards to the samples, shake them up to make the standards and samples fully absorbed, and then perform extraction and purification according to this method, using high performance liquid chromatography- Measured by tandem mass spectrometer, the recovery rate and precision are shown in Table 5-32
.
It can be seen from Table 5-32 that the recovery rate of this method is between 81.
Table 5-3 Experimental data of the recovery rate of 26 penicillins added indoors (n=10)
Related Links: Determination of 6 Penicillin Residues in Honey-Selection of Analysis Conditions