实验室残留分析质量控制指南(英文版）.doc

The program for Analysis Quality Control1.Foreward In order to keep in accordance with analysis quality of control, to ensure that the analysis residue results, which are accuracy and precision. The program has been issued. The program has prescribed the demand of the analysis quality control.According to Council Directive 93/256/EEC and Standard ISO/IEC/17025, the program has been issued 2.ScopeThe program applies to the laboratories that provide the analysis data on the residues material.3.Laboratory3.1Laboratorys quality systemThe laboratories that provide the analysis data on the residues material must obey the international standards (for instance ISO/IEC17025 etc.). Laboratorys quality system is established and availably worked. 3.2The responsibilities of the reference laboratories3.2.1The responsibilities are that guide the work of approved laboratories, assort with using the analysis methods. In order to rectify the deviation of the laboratory, it is necessary for the laboratory to organize the training course, comparative test, guide the analysis results.3.2.2 Assisting Chinese authorities in the monitoring program for residues issue and administer 3.2.3 Regularly organize comparative test between the laboratories3.2.4Training the analytical stuff3.2.5 Collecting information of the monitoring program for residues from china and abroad, providing annual summation from china and abroad for the assumed objects3.26 If it is necessary, provide the confirmatory test3.3 Approved laboratoryThe responsibilities of the approved laboratory are that assume the objects of the monitoring program for residues, join the relative training course, level test and comparative test.4. Sampling and disposal of sampleTo ensure each sample meet analysed demand, the samples should be representative, divided in two equal portions and put them into containers (bottle or bag). Samples should store under the nice condition after sampling, send them to the laboratories immediately. To keep in accordance with the components that will be analysed during the transportation.The container should be good sealing, it can prevent sample matrix changing. The laboratory stuffs should have a good communicated system with unit of sending samples or specified Transportation Company. It should be prevented that samples should not be arrived at the laboratories during the weekend and public holiday; otherwise it will not have any stuff to receive the samples and make the sample matrix change.The sample containers should have clear label, mark and code for each sample individually. The label should be tightness and hardly taking off from the container, and put on right place of the container。Some information should be relation with official sample form.When the laboratory received the samples, it must check the fettle and sealing of the samples, and the sample form. If the information is not consistent, please refund the samples back.To ensure the samples for the analysis, repeating and checking, and it will affect the results; it must focus on the materials that decompose in the biological samples particularly. The laboratory should have the documents processes, such as receive, dispose, register and store up. The Laboratory must divide the sample into two portions, one portion store for half year under suitable condition. The beginning time of the storage should account from finishing the sample test.5 Analysis methods5.1Defintion5.1.1Routine methods of analysisAccording to the law of inspection, quarantine and monitoring program for monitoring residues program, the laboratories use the methods. Routine methods must be approved by the laboratory, meet the relative provisions, use for screening and confirmatory. Screening Methods: are methods that are used to detect the presence of an analyte or for a high sample throughout are used to sift large numbers of samples for potential positives. The sensitivity meet demand of the residues. They are specifically designed to avoid false negative results.Confirmatory Methods: are methods that provide full or complementary information enabling the analyte to be identified unequivocally at the level of interest. The sensitivity meet demand of the residues as well. They are specifically designed to avoid false positive results.5.1.2 Interpretation of Resultsa) Positive Result: if the presence that must not be detected of the analysis in the sample is proved, the result is regarded as positive. For substances with an established maximum residue limit, the result of the analysis is considered as positive if the determined content of the identified analysis in the sample is greater than the MRLs.b) Negative Result: if the presence that must not be detected of the analysis in the sample, the presence that does not have in the sample is proved. For substances with an established MRLs, the content of the presence in the sample is lower than the MRLs, the result is negative.c) A negative result does not prove in case that the analysis is absent from the sample, or in case that the true content of the analysis is below the MRLs.5.2 Choosing the analysis methodThere are the Chinese national standard or the Chinese Vocation Standard.The recognized standard method, such as the methods has issued by international standard organization (ISO).The standard operation program should be admitted by authoritied management.The method that has been validated by the laboratory meet 5.4 provision and is approved by the relative process.5.3 Technical enquiring of the analysis method5.3.1 Screen Methoda) Limit of Detection: the LOD should be lowest for the banned presence. The LOD should be lower than the MRLs for the established presence.b) Specify: the result must be prescribed.c) Qualitative and Quantitative Method: depend on the analysis substance that belongs to prohibit or restrict. The false positive result should be accepted, however, the fewest false negative results should be obtained. d) Practicality: is suitable for the analysis large amount of samples, the analysis cost is cheap.5.3.2 Confirmatory methodsa) Trueness of quantitative methods: in the case of repeated analyses of a certified reference material, the guideline ranges for the deviation of the experimentally determined recovery corrected mean content from the certified value are as follows:Content (mg/kg) Range 1 -50% - +20% 1-10 -30% - +10% 10 -20% - +10% b) Precision of quantitative methods: the inter-laboratory Coefficient of Variation (CV) for the repeated analysis of a reference material under reproducibility conditions. The Horwitz equation is CV (%) = 2(1-0.5logc), where C is the content expressed as power of 10. Content (mg/kg) CV (%) 1 4510 32100 231000 16 For analyses carried out under repeatability conditions, the intra-laboratory CV would typically be between one half and two thirds of the above valuesc) Analytical Limits: for substances with an established maximum residue limit, the value of analytical limit plus 3 times of standard deviation for MRL of sample should be less than MRL. The method should be confirmed at three levels (analytical limit, MRL, two times of MRL). d) Specify: As far as possible, confirmatory methods must provide information on the chemical structure of the analysis. When more than one compound gives the same response, then the method cannot discriminate between these compounds. Methods based only on chromatographic analysis without the use of spectrometric detection are not suitable on their own for use as confirmatory methods. If a single technique lacks sufficient specificity, the desired specificity may be achieved by analytical procedures consisting of suitable combinations of clean-up, chromatographic separation(s) and spectrometric detection, such as GC-MS, LC-MS, IC/GC-MS, GC-infra-red detection, and LC-IC. 5.3.3 Calibration curvesWhen calibration curves are used for quantification:l The mathematical formula of the curve should be described.l The working range of the curve should be described.5.3.4 Susceptibility to interferenceFor all experimental conditions that could in practice by subject to fluctuation (stability of reagents, composition of the sample, PH, temperature) any variations that could affect the analytical result should be indicated. If the identification of the analysis should be confirmed by co-chromatography, in this case only one peak should be obtained, the enhanced peak height (or area) being equivalent to the amount of added analysis with GC or LC, the peak width at half-maximum, height should be within the 90-110% range of the original width, and the retention times should be identical within margin of 5%. For TLC methods, only the spot presumed to be due to the analysis should be intensified; a new spot should not appear, and the visual appearance should not change. 5.4 Method Quality Control5.4.1 Analytical methods must be validated or conformed thoroughly before it is carried out;5.4.2 The quality control procedures have been prescribed definitely, the staffs who have been examined and approved only could analyse the samples, calculate, record and check the analysis results.5.4.3 Control samples includes certified reference materials (CRM), or other laboratory reference materials were calibrated by the standard substances, which are recognized internationally. There are some recommended control samples as below:a) Blank sample that the analyte is absent.b) The content of real sample with target substances, which equals the MRLs, or little, exceeds the LODs, or LODs of the analytical methods.c) Real samples with target substances, which are above the MRLs, or the LODs, or LODs of the analytical methods.The quality control sample should use the incurred sample, if the incurred sample are not available, it could use spike sample.5.4.4 Analyzed each sample should be paralleled by analyzing the quality control sample, which include the three ones described on item 5.4.3 (sample a, sample b and sample c). If it is hard to get the three samples at one time, either sample a, b, or sample a, c are available for the test. Blind sample tests use to assess the abilities of inner-laboratory and inter-laboratory.5.4.5 The recovery, the linearity and the calibration curve should be checked by the spike samples (with positive control sample or internal standard). 5.4.6 The instruments should meet the requirement for analytical methods, and be calibrated and maintained regularly. 5.4.7 Data calculation should be presented in detail. The results must meet statistics quality control. If the results are calibrated by the value of recovery, the calibrated method must be described and stated clearly in the final result. 5.5 Criteria for methods of analysis which maybe used for confirmatory purposes only in combination with other methods The methods of analysis refer to use for confirmatory purposes only in combination with other methods.5.5.1 The quality requirement for immunology analysis (IA)a) It must prescribe the range of calibration curve. Normally it requires the range concentration. b) It must have six different concentrations at least.c) The parameters of quality control must be the same with the result prior. For instance: non-specific combination and parameters of calibration curve.Analyzed each sample should be paralleled by analyzing the quality control sample. The concentration of the quality control sample should be: zero, lower, higher concentrations in the construction of the curve. The result should be the same with the result prior. 5.5.2 Criteria for the determination of a non-specific analyte using HPLC or GCa) The analyte should elute at the retention time that is typical for the corresponding standard analyte under the same experimental conditions.b) The nearest peak maximum in the chromatogram should be separated from the designated analyte peak by at least one full width at 10% of the maximum height.c) The analyte could use spiking or two columns of different polarity at least; it will obtain the further information.5.5.3 Criteria for the determination of an anlayte using TLCa) The RF values of the analyte should agree with the RF values of the standards within3%.b) The visual of the analyte should be indistinguishable from that of the standard.For spots of the same colour the center of nearest spot should be separated from the center of the spot of the analyte by at least half the sum of the spot diameters.The analyte could use spiking or 2-D TLC; it will obtain the further information.5.6 Criteria for methods of an anlayte, which may be used for confirmatory purposes5.6.1 Criteria for the determination of an analyte using LC-spectrumIt must meet the criteria of 5.5.2.The absorption maximum in the spectrum of the analyte should be at the same wavelengths as those of the standard analyte within a margin determined by the resolution of the detection system. For diode array detection this is typically within 2 nm.The spectrum of the analyte above 220 nm should not be visually different from the spectrum of the standard analyte for those parts of the two spectra with a relative absorbance10%.If the method has not combined with other methods, the analyte must use spiking when the result is confirmed.5.6.2 Criteria for the determination of an analyte using TLC-spectruma) It must meet the criteria of 5.5.3.b) The absorption maximum in the spectrum of the analyte should be at the same wavelengths as those of the standard analyte within a margin determined by the resolution of the detection system.The chromatography of an analyte should be the same with those of the standard analyte.If the method has not combined with other methods, when the confirmatory of an analyte must use spiking or 2-D TLC. 5.6.3 Criteria for the determination of an analyte using GC MASS a) Criteria for the determination of an analyte using GC.It must meet the criteria of 5.5.2. An internal standard should be used if a material suitable for this purpose is available. It should preferably be stable isotope-labelled forms of the analyte, if it hard to get it, it will use a related standard with a retention time close to that of the analyte. The ratio of the retention time of the analyte to that of the internal standard, the relative retention time of the analyte, should be the same as that of the standard analyte in the appropriate matrix, within a margin of 0.5%.If the confirmatory method does not use internal standard, it will use spiking.b) Criteria for lower resolution Mass As a screen method it has a maximum intensity characteristic fragment ion at lest. As a confirmatory method, it should be determined 4 intensities characteristic fragment ions at lest. When the method has been used, the molecular produce the characteristic fragment ions that are less than four. It will take two different tests of derivatision /ionization independently at least. Each test produces 2 or 3 characteristic fragment ions. The result should be confirmed under this cond