方法验证（详细参数,英文）
Category I Category III Category IV Definition Validation Procedure Acceptance Criteria Verification
Target of analyticaleverywhere
methods Assay
Impurity
Quantitative
Impurity
Limit Tests
Dissolution Identification
Accuracy Yes Yes**No The nearness of a measured
value to the true value
Spike certain amount and calculate the
percentage recovery (3
concentrations/three replicates, minimum
9 determinations over minimum of three
英汉在线翻译器concentration levels per ICH).
For Assay: 5 Conc. X 3 replicates
98% - 102%
For Impurity: 3 Conc. X 3 replicates
85% - 115%
*
Precision Yes Yes No Yes No Cloness of agreement
between a ries
measurements
Repeatability, Intermediate precision, and
reproducibility
See Below for Detail Yes
Repeatability Yes Yes No Yes No Measure of the precision under
the same operationconditions
over a short interval of time
(with the same equipment)
%RSD (3 concentrations/three replicates,
minimum 9 determinations over minimum
of three concentration levels, or minimum
of 6 determinations at 100% of the test
concentration per ICH
Assay (Category I) NMT 2%
Impurity (Category II) NMT 15% or
Bad on repeatability of instruments
Yes
imf是什么意思Intermediate Precision Yes Yes No Yes No
Measure the variation within
the same laboratory, including
Day-to-day variation, analyst
variation, and equipment
variation
SD, %RSD, and Confidence interval
The obtained variability that is in the
same range or less than repeatability
variation.
Yes
Reproducibility Yes Yes No Yes No
Measures the precision
between laboratories (Method
transfer between laboratories)
Means of repeatability data
The means of the two laboratories
存钱英语are not significant different from each
other
Yes
Specificity Yes Yes Yes*Yes
The ability to asss
unequivocally an analyst in the
prence of componenets
thatmay be expected to be
prent
1. When Impurities are available:
1.1 Assay Method: Comparing test results
between Sample with Impurities and
sample without impurities.
1.2 Impurities Method: Spike drug
substance with the appropriate level of
impurities (LOQ);
2. When Impurities are not available,
demonstrated specificity by comparing
the test results of samples containing
single是什么意思
impurities to a cond well
characterized procedure or other
validated procedure, should include
samples stored under relevant stress
conditions:
2.1 Assay method: The two results should
be compared;
2.2 Impurities Method: The impurity
profiles should be compared and peak
purity check (using DAD or MSD) should
matchesbe performed;
1. When Impurities are available:英语演讲范文
1.1 Assay Method: Impurities peaks
need to be resolved from the analyte.
Impurities do not need to resolved
from each other;
1.2 Impurities Method: impurities are
determined with appropriate
accuracy, precision, and peration
of the impurities individually;
how interesting2. When Impurities are not
available
2.1 Assay method: The two results
should be compared;
2.2 Impurities Method: The impurity
profiles should be compared and
peak purity check (using DAD or
MSD) should be performed to shown
that the analyte chromatographic
peak is not attributable to more than
one component
灰姑娘剧本*
Detection Limit (LOD)No No Yes*No The lowest amount of analyte
in a sample that can be
detected, but not necessarily
quantitated, under the stated
experimental conditions.
1. For noninstrumental procedure:
generally determined by the analysis of
针线包英文samples with known concentration of
analyte;
2. For instrumental procedures: The
detection limit is shown to be sufficiently
low by the analysis of samples with known
concentrations of analyte above and
below the required detection level.
Usually at least 3-5 times lower than the
limit (20% to 33% of the required limit).
Prepare veral (at least 5, recommend
7) samples at the LOD level and test.
1. Visual evaluation for
noninstrumental procedures and
instrumental procedures;
2. Signal-to-noi ratio of 3:1 at least;
3. LOD = 3σ/S, where σ is the
standard deviation of multiple blank
samples respon and the S is the
slope of the calibration curve. Usually
the RSD of LOD level is NMT 10%
for HPLC method
No
Quantitation Limit
(LOQ)No Yes No*No
A characteristic of quantitative
assays for low levels of
compounds in sample
materices, such as impurities
in bulk drug substances and
