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9.
2.
1.
8 Linearity range and lower detection limit
Zearalanol formulated, corn Zearalanone and hexoestrol standard concentrations were 1.
25ng / mL, 2.
5ng / mL, 12.
5ng / mL, 25ng / mL, diethylstilbestrol , dienes female phenol standard concentrations were 2.
5ng/mL, 5.
0ng/mL, 25ng/mL, 50ng/mL mixed standard solutions, under the test conditions of this method, inject 50μL for determination, and use the peak area corrected by the internal standard to compare each test in the standard solution The concentration of the components is plotted, and each target is in a linear relationship within the detection range.
The linear equation and correlation coefficient are shown in Table 9-9
.
Table 9-9 Linear equation and correlation coefficient of the measured object
9.
2.
1.
9 Method recovery and precision
Use bovine muscle samples that do not contain zearalenol, zearalenone, diethylstilbestrol, diethylstilbestrol, and hexestrol for addition recovery and precision testing.
After adding different concentration standards to the samples, perform sample preparation according to this method.
Purification and determination, the analysis results are shown in Table 9-10
.
It can be seen from the results in Table 9-10 that the detection limit of the equivalent method is 0.
Bovine liver and kidney and muscle tissue samples containing no zearalenol, zearalenone, diethylstilbestrol, diethylstilbestrol, and hexestrol were used for the recovery rate and precision test of the addition to verify the applicability of the method
.
After adding different concentration standards to the samples, sample preparation, purification and determination are carried out according to this method.
Table 9-10 5 kinds of hormones and metabolites added recovery rate experimental data (n=10)
Table 9-11 Experimental data of adding recovery rate (%) in different matrices
9.
2.
1.
10 Repeatability and reproducibility
Under the 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, the test results should be discarded and the determination of two individual tests should be completed again
Table 9-12 Content range and repeatability and reproducibility equation
Related links: Selection of analysis conditions for determination of zearalenol, zearalenone, diethylstilbestrol, hexestrol, and diethylstilbestrol residues in bovine liver, kidney and muscle tissues