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4.
2.
2.
8 Linearity range and lower limit of determination
Mix 0μg/L, 0.
05ug/L, 0.
1μg/L, 0.
5μg/L, 1.
0μg/L, 2.
0μg/L and 5.
0μg/L of mixed standard working solution with water.
Each milliliter of the mixed standard working solution contains 3ng deuterated chloramphenicol
.
Measure under the selected chromatographic and mass spectrometry conditions, and use the ratio of the peak area of the measured component of the standard working solution to the peak area of the internal standard substance of the standard working solution to the concentration of the measured component of the standard solution working solution and the internal standard substance of the standard working solution The ratio of the concentration is used as a linear regression curve
Table 4-11 Quantitative ion pairs, linear equations, and correlation coefficients of chloramphenicol, thiamphenicol and florfenicol
4.
2.
2.
9
Method recovery and precision
Supplemental recovery and precision experiments were carried out with chloramphenicol-free muscle, fish, shrimp and liver samples
.
The results of recovery and precision of addition are shown in Table 4-12
Table 4-12 Addition recovery rate and precision experimental results (n=10)
It can be seen from Table 4-12 that the average recovery rate of chloramphenicol , thiamphenicol and florfenicol in muscle, liver, fish and shrimp meat is between 0.
1~4.
0ug/kg and 77.
3%~118.
0%.
, The relative standard deviation is 4.
0%~16.
4%
.
4.
2.
2.
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 individual tests should be completed again.
Determination
.
Under the reproducibility test conditions, the absolute difference between the two independent test results obtained does not exceed the reproducibility limit (R)
Table 4-13 The content range and repeatability and reproducibility equation of chloramphenicol, thiamphenicol and florfenicol (substrate is animal muscle)
Table 4-14 The content range and repeatability and reproducibility equation of chloramphenicol, thiamphenicol and florfenicol (substrate is animal liver)