Proceedings of the International Cyanide Detection Testing Workshop

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• Statistics: Statistical techniques are employed to evaluate accuracy, precision, linear range, limits of detection and quantifi cation, and measurement uncertainty. 5.3.1.3 General Validation Protocol Guidance The following provides guidelines that should be used to determine method performance characteristics: • Quantitative measurements, e.g. determine limit of quantitation (LOQ), linear response. Minimally need LOD • Prepare and analyze spiked blanks, matrix samples of known concentration utilizing at least three different concentration levels: low, medium, high based on the intended use of the method. These samples are carried through the complete sample preparation procedure, extraction and analytical steps of a particular method. Matrix effects can also be assessed with these samples. Accuracy and precision are calculated from these results; data will also evaluate robustness of the method resulting from changes in the sample matrix. (Note: Proper certifi ed reference materials and reference standards are used when available.) • Assure that adequate sample replicates are performed and that results from replicate measurements of each analyte are compared. • Analyze blanks (reagent and matrix) and compare these results to the reported limit of detection • Evaluate interferences: spectral, physical, chemical or memory by analyzing samples containing various suspected interferences in the presence of the measurand. 5.3.1.4 Validation of Methods (Original, New or Modifi ed), should include but not be limited to matrix extensions and platform changes. • In cases where the sample preparation and/or the extraction procedure/analytical method is modifi ed from the existing test procedure and protocol, the new method should demonstrate that the modifi cations do not adversely affect the precision and accuracy of the data obtained. • In order to implement the modifi ed method, the standard or existing method is fi rst performed. The modifi ed method is then verifi ed against the original method validation protocol as defi ned in section 5.3.1.3. • For original or new methods the authors should pick a validation level that is suitable for their situation as defi ned in section 5.4. 5.4 Levels of Validation 5.4.1 It is the responsibility of the individual network to determine the level of validation that is acceptable for use on the particular method. 5.4.2 This section references four levels of validations: Level One: The method is tested in one laboratory for one or more analytes and one or more matrices. The laboratory would select a limited number of key characteristic to evaluate the method performance. (See tables 1, 2, and 3 for specifi c details for level 1 validation) 68
Level Two: The method should be validated in a single laboratory. (See tables 1, 2, and 3 for specifi c details for level 2 validation) • “Wherever possible and practical a laboratory should use a method of analysis that has had its performance characteristics evaluated through a collaborative trial conforming to an international protocol. Page 844 Pure and Applied Chemistry, 2002, 74” • “Single-laboratory validation requires the laboratory to select appropriate characteristics for evaluation from the following: applicability, selectivity, calibration, accuracy, precision, range, limit of quantifi cation, limit of detection, sensitivity, and ruggedness. Page 845 Pure and Applied Chemistry, 2002, 74.” This is similar to the MARLAP tiered project method validation approach for radio analytical methods. Level Three: The method should be validated by testing the applicable performance characteristics from a single laboratory validation study using two to seven labs with one or more matrices. (See tables 1, 2, and 3 for specifi c details for level 3 validation) Level Four: The method is tested using the criteria for a full collaborative study. The study should examine bias, recoveries, applicability, interference, method comparison, calibration procedures and all applicable performance characteristics examined in a single laboratory validation. (See tables 1, 2, and 3 for specifi c details for level 4 validation) • For a single type of substance at least 5 materials (test samples) must be used; only when a single level of specifi cation is involved for a single matrix may this minimum required number of materials be reduced to 3. Page 334, Pure and Applied Chemistry, 67, No. 2, 1995. • At least 8 laboratories should report the results for each matrix; only when it is impossible to obtain this number may the study be conducted with fewer, but with an absolute minimum of 5 laboratories. Page 335, Pure and Applied Chemistry, 67, No. 2, 1995. • The entire protocol is outlined in the article “Protocol for the Design, Conduct, and Interpretation of Method-Performance Studies, Pure and Applied Chemistry, 67, No. 2, 1995, 331-343. 69
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Proceedings of the International Cy
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Proceedings of the Cyanide Detectio
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ACKNOWLEDGEMENTS The Proceedings of
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PREFACE The International Cyanide D
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EXECUTIVE SUMMARY The International
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ATCA) in homogenized fi sh tissue m
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Validation of the ISE method applie
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Importing countries should also req
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INTRODUCTION Cyanide fi shing is a
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through the implementation of a net
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Working Group 2 The Export Working
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o o o o Can the U.S. require verifi
Page 27 and 28: Polymeric membrane based ion select
Page 29 and 30: Goal 2: Provide recommendations on
Page 31 and 32: hands-on training that develops a d
Page 33 and 34: Goal 3: Identify research needs to
Page 35 and 36: Working Group 1 Participants Bob KO
Page 37 and 38: estimated at roughly 3 to 5 days. H
Page 39 and 40: Goal 2 : Identify steps, agreements
Page 41 and 42: 3) certifi cate, but tests positive
Page 43 and 44: Report from Working Group 3 The Par
Page 45 and 46: No. of Shipments 6,000 5,000 4,000
Page 47 and 48: Goal 3: Provide a recommendation wi
Page 49: Working Group 3 Participants Eric P
Page 53 and 54: Introduction Since the early 1960
Page 55 and 56: ainbow trout exposed to 40 mg SCN -
Page 57 and 58: Blennies, which were net-caught and
Page 59 and 60: electrical potential (similar to an
Page 61 and 62: in the Philippines under contract w
Page 63 and 64: endorsing the IMA’s use of the IS
Page 65 and 66: The intended products from the rese
Page 67 and 68: WPCF 1992, 1998). Both of these stu
Page 69 and 70: ASTM (1997) Standard test methods f
Page 71 and 72: Kuegsen, M., Kloock, J.P., Knobbe,
Page 73 and 74: Philippines. In Proceedings from th
Page 75 and 76: 3) 4) 5) 6) the metabolism of cyani
Page 77: or new matrices. 5.2.3 Modifi catio
Page 81 and 82: of cyanide exposure and to identify
Page 83 and 84: Special considerations for the anal
Page 85 and 86: tissue samples indispensable. Altho
Page 87 and 88: y reduction and subsequent separati
Page 89 and 90: can also be used for analysis of cy
Page 91 and 92: thiocyanate in saliva and serum bas
Page 93 and 94: are many discrepancies in the liter
Page 95 and 96: Table 3. Analytical Methods to dete
Page 97 and 98: Poisoning, In Textbook of military
Page 99 and 100: (70) Odoul, M., Fouillet, B., Nouri
Page 101 and 102: V. (1975) Stable reagents for the c
Page 103 and 104: (159) Felscher, D. and Wulfmeyer, M
Page 105 and 106: Purpose of this Document The purpos
Page 107 and 108: day. One cyanide tablet (2 g) is mi
Page 109 and 110: 10-90% following exposure to cyanid
Page 111 and 112: existing cyanide detection methods
Page 113 and 114: - Plasma lactate — elevated plasm
Page 115 and 116: Method Advantages Disadvantages Hig
Page 117 and 118: Paper Method Matrix Detection Limit
Page 119 and 120: Table 4 lists experts identifi ed t
Page 121 and 122: X Jerry Thomas CDC Em Steve Borron
Page 123 and 124: References Barber, C. and Pratt, V.
Page 125 and 126: Rates of Recovery. Environmental Ma
Page 127: COUNTRY REPORTS
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The first three of these destructiv
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enforcement is minimal. There is an
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1. Management/guidance to the Minis
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in Vietnam now and requires more ef
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Figure 2: Administrative structure
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References Baquero, J. (1999) Marin
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Acronyms • CDT • Cyanide Detect
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Law/Ordinance/Decree /Decision 52/2
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of samples required for analysis. U
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Field test kit. BFAR recognizes the
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Political Will Having planted the s
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gravely by fi shing communities. Th
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ecome the partner and counterpart o
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Ion-Selective Electrodes for Cyanid
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References Alban, J., Manipula, B.E
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levels with mV readings recorded as
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Trends Determined by Cyanide Testin
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Implementing agencies: • Quaranti
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APPENDIX
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1:30 Overview of and Potential Cyan
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Kristine Johnson Director Kingfi sh
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Assessment of U.S. Role in Trade: U
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