Proceedings of the International Cyanide Detection Testing Workshop

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Validation Methods for the Determination of Cyanide and Cyanide Metabolites in Coral Reef Fishes Robert Kobelski National Center for Environmental Health Centers for Disease Control and Prevention rmk9@cdc.gov The consensus of the Working Group was that there exist serious gaps in the understanding of the metabolism and elimination of the cyanide anion and its major metabolites in fi sh. Without a better understanding of these processes the implementation of an exposure assessment method that would meet legal requirements would be diffi cult. The recommendation of the Working Group is that a research program be designed to generate the data necessary to determine the determine the availability of cyanide and its metabolites for exposure assessment versus the time involved with the local collection of fi sh, their transport to a fi xed site laboratory prior to export and their arrival at the import destination prior to the implementation of an analysis method at any point in the delivery chain. Background In a number of locations both ornamental and live food fi sh are captured using techniques such as stunning with an aqueous solution containing the cyanide anion (CN - ). This technique is destructive to the reef, the individual fi sh and the sustainability of the population and is illegal in Indonesia, the Philippines and Vietnam. To determine if fi sh are captured using this destructive technique there must be a forensically supportable analysis for cyanide exposure in reef fi sh implemented in a timely fashion after capture of the fi sh. The length of time between capture and delivery of the fi sh to a capable laboratory can range from fi ve to fourteen days. For a laboratory analysis to be viable the analyte must be stable and at elevated levels in the sample long enough for the sample to be delivered to the laboratory and for the analysis to be conducted. Data from mammals suggests that the cyanide anion is readily metabolized to thiocyanante (SCN - ) and 2-aminothiazoline-4-carboxylic acid (ATCA), with a half-life of approximately one hour. If metabolism in fi sh is similar there would not be an elevated level of cyanide in a fi sh when it reached the laboratory site For there to be an elevated level of cyanide after fi ve days the half-life would have to be approximately 10 hours, but this toxicokinetics parameter has not been determined. To determine what analyte can be targeted for forensic analysis the following research needs to be conducted: 1) the half-life of cyanide in fi sh has to be determined and the variation in half-life with respect to different species must be defi ned, 2) the half-life of thiocyanate, the major metabolite of cyanide, in fi sh must be determined as well as the specie-to-specie variation in half-life 64
3) 4) 5) 6) the metabolism of cyanide to ATCA must be demonstrated and if this is a metabolic pathway for fi sh the half-life of ATCA must be determined as well as the specie-to specie variation in half-life, the background level of cyanide in fi sh must be determined, if it is above the limit of quantitation (LOQ) of the analysis technique, to defi ne when an elevated level due to cyanide exposure has been encountered. The background level of thiocyanate in fi sh must be determined, to defi ne if an exposure to cyanide will result in a statistically meaningful elevation of background thiocycante The background level of ATCA must be determined, if it is above the LOQ of the analysis technique, to defi ne when an elevated level due to cyanide exposure has been encountered. To perform this research, validated methods for the determination of cyanide, thiocyanate and ATCA in homogenized fi sh tissue must be used. These methods must demonstrate adequate sensitivity, specifi city, accuracy and precision as determined by the “fi t for purpose” concept. 3. Outline of Validation Procedure: 3.1 Method validation is a process by which a laboratory confi rms by examination and the provision of objective evidence that the particular requirements for specifi c use are fulfi lled. It serves to demonstrate that: 3.1.1 The method can detect, identify and quantitate an analyte(s): • In all matracies to be analyzed • With a demonstrated sensitivity, specifi city, accuracy, reproducibility, ruggedness and precision to ensure that results are meaningful and appropriate for decision making by the receiving network. 3.1.2 The method will function reliably for its intended purpose as defi ned by the network. 3.2 The method developer validates a method by conducting experiments to determine or verify a number of specifi c performance characteristics that serve to defi ne and quantify method performance. 4. Reference(s): 4.1 Food and Drug Administration, Laboratory Manual, ORA Laboratory Procedure, Volume II, ORA-LAB5.4.5, Methods, Method Verifi cation and Validation 4.2 International ANS/ISO/IEC Guide to the Expression of Uncertainty in Measurement, 1995 4.3 International ANS/ISO/IEC Guide 2 (VIM), 2004 4.4 International ANS/ISO/IEC Guide 8402, Quality Management and Quality Assurance 65
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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
Page 23 and 24: Working Group 2 The Export Working
Page 25 and 26: 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: Philippines. In Proceedings from th
Page 77 and 78: or new matrices. 5.2.3 Modifi catio
Page 79 and 80: Level Two: The method should be val
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.
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Rates of Recovery. Environmental Ma
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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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