OMB Meeting Book_9-11-14

Vitamin A & E MLT Protocol For ERP Use Only DO NOT DISTRIBUTE

d) The stock calibration curve should be prepared once and the 6 point curve diluted freshly on each day.

e) Due to the variability in relative levels (of the analyte) in each sample, the concentration range of the calibration solutions should be prepared as described in the method.

f) The Reference Standard Template in Appendix 3 should be used to record reference calibration weights and UV absorbance values and to calculate the calibration standard concentrations.

Reporting Results

a) As noted above, record all actions, observations, and deviations to the method.

b) When results are below the limit of quantitation, report the limit of quantitation regardless of value.

c) All results and calculations should be reviewed by the laboratory supervisor or manager.

d) Final results should be summarized in the results sheets in Appendix 4 .

Outliers

a) If analytical results appear unreasonable (values outside the range given in the protocol’s applicability statement, for example) investigate possible cause immediately, first by checking for transcription and calculation errors. Call the Study Director to discuss suspicious values. If the Study Director indicates the value may be an outlier, review the suspect values by recalculation, re-analysis and/or preparation of new standards.

b) Since collaborators have no basis for judging whether a value is an outlier, all results should be communicated to the Study Director as soon as possible .

c) Results shall be communicated to the Study Director by e-mail.

d) Correctable Outliers – The most frequent cause of correctable outliers are:

 Incorrect calculations and arithmetic errors.

 Errors in reporting, such as transposition of numbers, misplacement of the decimal point, or use of the wrong units.

 Incorrect standards due to weighing or volumetric errors

 Contamination of reagents, equipment, or test materials.

Upon Completion

Upon completion of the analysis of the test materials, all relevant raw data should be returned to the Study Director. A pre-addressed return envelope will be provided for your convenience. All results and analysis forms should be sent by e-mail including the excal result files. Please keep a copy of all documents for yourself.

The following should be included:

a) All original chromatograms obtained from the instrument system checks, practice sample analysis, and test material analysis. Separate raw data by analysis set. All chromatogeams should be clearly identified with sample ID or standard concentration. All sets of chromatograms should be reviewed and signed. Should re-integration be required, include original and re-integrated chromtograms. All calibration curve raw data, including the correlation coefficient (r) should be included.

b) Analysis reports and documents containing any attached notes on the preparation of all reagents and solutions, and notes on all observations and deviations to the method.

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