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Scope:
3. Limit tests.
Procedure:
b. Selectivity:
e. Assay Precision:
f. Limit of Detection:
g. Limit of Quantitation:
The LOQ is the minimum level of the analyte in the matrix that can be
quantitated at the 95 percent confidence level. It is a parameter of the
quantitative assay for low levels of compounds in sample matrices
such as impurities in bulk drug substances and degradation products in
finished pharamceuticlas. It is the lowest concentration of analyte in a
sample that can be determined with acceptable precision and accuracy
under the stated experimental conditions.
h. Ruggedness:
i. Robustness:
* Store under
a. Prepare standard solution containing 50, 75, 100, 125 and 150
percent of the working concentration of analyte by dilution of the 10
times the working concentration standard, prepared as directed in
5.4.1.1. according to the following table:
c. The signal (e.g., peak area) obtained for each solution is plotted
against its corresponding theoretical concentration and a liner
regression analysis is performed on the 5 coordinates. The resulting
plot should be linear for each analyte at least 0.999 since it describes
the line of most accurate fit to the data or potential assay bias.
observed signal
Response factor = Kt = concentrat ion (mg/mL)
residual
& residual = Observed signal x 100
Linearity
Standards mL of mL of Final
(% Working 10 x 10 x Volume
Concentration Placebo Standard (mL)
)
50 10 5.0 100.0
75 20 15.0 200.0
100 10 10.0 100.0
25 20 25.0 200.0
The RSD for the measurement precision is no more than 2.0 and the
recovery is not more than ± 2.0 percent relative to the freshly prepared
calibration standard or standards.
7. Assay Precision:
d. The RSD of the 6 results for each analyte should not be more
than 2.0.
8. Limit of Detection:
The LOD of the analytical method is determined by comparing the test results
obtained from samples with known concentrations of analyte against those of
blank samples and establishing the minimum level of analyte that can be
reliably detected. A signal-to-ratio of 3:1 is acceptable.
9. Limit of Quantitation:
10. Ruggedness:
11. Robustness:
III. Precision
III. Precision
III. Precision
III. Precision
III. Precision
a. Summary:
c. Discussion:
1. Protocol:
2. Report: