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GB 5009.295-2023: National food safety standard - General rules for verification of chemical analysis methods
GB 5009.295-2023
GB
NATIONAL STANDARD OF THE
PEOPLE’S REPUBLIC OF CHINA
National Food Safety Standard -- General Principles for
Validation of Chemical Analysis Methods
ISSUED ON. SEPTEMBER 06, 2023
IMPLEMENTED ON. SEPTEMBER 06, 2024
Issued by. National Health Commission of the People's Republic of China;
State Administration for Market Regulation.
Table of Contents
1 Scope... 3
2 Terms and definitions... 3
2.1 Method validation... 3
2.2 Qualitative method... 3
2.3 Quantitative method... 3
2.4 Concentration paid attention to... 3
2.5 Specificity... 3
2.6 Detection limit... 4
2.7 Limit of quantification... 4
2.8 Measuring range... 4
2.9 Accuracy... 4
2.10 Repeatability... 4
2.11 Reproducibility... 4
2.12 Stability... 4
2.13 Robustness... 4
2.14 Intermediate precision... 5
2.15 Linear range... 5
2.16 Detection probability... 5
3 General requirements for validation of chemical analysis methods... 5
3.1 Selection of performance parameters... 5
3.2 Selection of representative foods... 6
3.3 Validation sample requirements... 6
3.4 Data processing requirements... 7
4 Validation of performance parameters of chemical analysis methods... 7
4.1 Validation of method performance parameters... 7
4.1.1 Specificity... 7
4.1.2 Detection limit... 8
4.1.3 Limit of quantitation... 9
4.1.4 Measuring range... 9
4.1.5 Accuracy... 10
4.1.6 Precision... 11
4.1.7 Stability... 12
4.1.8 Robustness... 13
4.2 Validation of method equivalence... 13
4.2.1 Validation requirements... 13
4.2.2 Validation method... 13
Annex A Classification of food samples for validation of chemical analysis methods
... 15
Annex B Robustness test of the method... 18
National Food Safety Standard -- General Principles for
Validation of Chemical Analysis Methods
1 Scope
This Standard specifies the general requirements for the validation of national food
safety standard -- chemical analysis methods.
This Standard is applicable to the validation process during the development and
revision of national food safety standard -- chemical analysis methods.
2 Terms and definitions
2.1 Method validation
Test activities that provide objective and valid evidence to confirm that the performance
parameters of an analytical method meet the intended use of the method.
2.2 Qualitative method
An analytical method that identifies the presence or absence of a target analyte in a
sample based on its specific properties.
2.3 Quantitative method
An analytical method that determines the concentration or amount of target analytes
under conditions that meet specified precision and accuracy.
2.4 Concentration paid attention to
The concentration that is decisive for determining whether the target analyte in the
sample meets the requirements of regulations or standards.
2.5 Specificity
The ability of an analytical method to distinguish between target analytes and
interfering substances.
2.14 Intermediate precision
In the same laboratory, over a long period of time (pay attention to small changes in test
conditions, such as temperature, humidity, light, etc.), the precision of independent
measurement results obtained by using the same method to test the same sample.
2.15 Linear range
Under a certain level of significance, a linear calculation model is used to define the
relationship between instrument response and concentration (or amount), which
conforms to the interval between the lowest concentration (or amount) and the highest
concentration (or amount) of the calculation model.
2.16 Detection probability
The probability that an analytical method will detect the target analyte at a specified
concentration and confidence level.
3 General requirements for validation of chemical analysis
methods
3.1 Selection of performance parameters
3.1.1 For qualitative methods, intra-laboratory and inter-laboratory validation
parameters shall include method specificity and detection limit.
3.1.2 For quantitative methods, laboratory validation parameters shall include method
specificity, detection limit, quantitation limit, measurement range, accuracy, and
repeatability. Interlaboratory validation parameters shall include the detection limit,
quantification limit, determination range, correctness and reproducibility of the method.
3.1.3 When the analysis method is sensitive to small changes in test conditions such as
temperature, humidity, and lighting, the robustness of the method shall be examined,
and the intermediate precision index shall be calculated.
3.1.4 When there are two or more methods with the same applicable scope for the same
target analyte, the equivalence of the different methods needs to be validated.
3.1.5 When literature data on the stability of a reference material are lacking, its stability
shall be validated.
3.1.6 Selection of intra-laboratory and inter-laboratory validation parameters is shown
use of the method.
b) For a sample matrix, at least 3 concentration levels are required, including the
lowest concentration, the middle concentration (generally the concentration of
concern) and the highest concentration of the method's determination range. Their
uniformity and stability are tested.
3.3.4 When selecting a standard addition sample for validation, the validation sample
can be prepared as follows.
a) The sample matrix shall be selected to be representative and meet the intended
use of the method.
b) For a sample matrix, at least 3 concentration addition levels are required,
including the lowest concentration, the middle concentration (generally the
concentration of concern) and the highest concentration of the method
determination range.
3.4 Data processing requirements
All laboratory validation data need to be subjected to outlier testing and statistical
analysis. The analysis method can use statistical methods such as Grubbs test. After
eliminating outliers through technical analysis, the number of laboratories and the
amount of validation data shall meet statistical requirements.
4 Validation of performance parameters of chemical analysis
methods
4.1 Validation of method performance parameters
4.1.1 Specificity
4.1.1.1 Validation requirements
The ability of the analytical method to differentiate between the target analyte and other
substances shall be validated. There shall be no interference factors (signals,
interference peaks, etc.) that lead to errors in the identification of the target analyte and
affect the accuracy of quantitation.
4.1.1.2 Validation method
Analyze representative samples that match the scope of the method. Check whether
there are any interferences (signals, peaks, etc.) that lead to incorrect identification of
the target analytes and/or affect accurate quantitation. A certain concentration of
substances that may interfere with the identification and/or quantification of the target
analyte is added to a representative sample and then analyzed. Check whether these
interfering substances can be effectively identified.
4.1.2 Detection limit
4.1.2.1 Validation requirements
The detection probability of the target analyte at the detection limit level shall be no
less than 95% (at the 95% confidence level). The detection limit needs to be
independently validated for each representative sample matrix.
4.1.2.2 Validation method
4.1.2.2.1 Estimation method
Methods for estimating detection limits includ...