Proceedings of the International Cyanide Detection Testing Workshop

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have all provided insight into the verifi cation of cyanide exposure from analysis of biological samples. Table 3 provides a comparison of analytical techniques for analysis of cyanide or its metabolites based on sensitivity, specifi city, sample size, capacity, expertise necessary to perform the method, and cost. Some other key pieces of information should also be considered prior to choosing a method to perform: 1) Was preservation of cyanide and its metabolites during storage addressed?; 2) Were typical interferences for the biological matrix of interest removed?; 3) Were analysis procedures that could result in the loss of cyanide or its metabolites used (i.e., heating or acidifi cation)? For the analysis of cyanide, the largest inconsistency in the literature is analysis with different preservation techniques. Regardless of the analytical method, a preserving technique needs to be considered so that accurate concentrations of cyanide can be found (75, 87, 112, 123, 128, 197-200). If cyanide is analyzed, biological samples should be collected and analyzed as soon as possible for confi rmation or refuting cyanide exposure. One also needs to consider that all biological samples will contain endogenous levels of cyanide (and its metabolites). Therefore, baseline levels of the analyte measured should 84 be known prior to concluding an exposure occurred. Problems with direct analysis of cyanide, including short half-lives, artifactual formation of cyanide, and interconversion of cyanide and thiocyanate, contribute to diffi culties in the analysis of cyanide for all analytical methods designed to determine cyanide in biological samples. While cyanide is most often analyzed to determine cyanide exposure, one should consider using analytical techniques that analyze for cyanide metabolites as well as those that analyze for cyanide directly. Although cyanide metabolites may offer longer halflives, they also have a number of drawbacks. For thiocyanate, the main drawback is large and variable background concentrations in biological samples. Other disadvantages include are interconversion of cyanide and thiocyanate, and the use of thiocyanate by other biological processes not directly related to cyanide metabolism. For ATCA and cyanide-protein adducts, the main drawback is the limited amount of research available on toxicokinetics and relationships of these metabolites to cyanide exposure. Care should be taken when choosing an analytical method to consider not just the parameters of the analytical method but also the toxicokinetics of cyanide and its metabolites.
Table 3. Analytical Methods to determine cyanide and its metabolites in biological fl uids. a Techniqueb Sub-category Analytec Matrices Sensitivityd Specifi cityd Sample Sized Capacityd Expertised Costd Refs. (41, 44, 60, 61, 76, 77, CN, SCN, Blood, Urine, 82, 87, 89, 101-105, UV-Vis None Low Low 0.5-1 mL Medium Low Low ATCA Saliva 108, 109, 115-119, 123, 178, 179) Fluorescence CN Blood Medium Medium 0.5-1 mL Medium Medium (77, 110-114, 124) Low- Medium Luminescence Medium 3 μL Medium Medium Low (180) Medium- High CN Blood Chemiluminescence (15, 21, 90, 130-137, 182, 183, 185-187, 201, 202) Very Low -Low Low Medium- High 1-5 mL Medium- High Medium- High Blood, Saliva, Tissue None CN, SCN Electrochemistry (127) Medium- High Medium 1 mL Low Medium Medium- High AA Indirect AA SCN Blood, Saliva (15) Very Low -Low Low Medium- High 1-5 mL Medium- High Medium- High Blood, Urine, Saliva Biosensor None CN, SCN Medium (89, 95, 160, 166) Medium- High High 10-100 μL RP-HPLC UV CN, SCN Blood, Urine Medium High (37, 84, 88, 93, 159, 163, 164) High High Medium 10-100 μL High High Blood, Urine, Saliva CN, SCN, ATCA RP-HPLC fl uorescence Medium (162, 165, 168) Medium- High High 10-100 μL High Medium- High SCN Urine High Very High High (80) 10-100 μL Extremely High CN Blood Very High RP-HPLC electrochemical RP-HPLC mass spectrometric 85 LC (29) Extremely High Extremely High Low 10-100 μL Extremely High Extremely High Blood CN-protein adduct RP-HPLC MS-MS Medium High 1-100 μL High High Medium (97, 167, 169) Blood, Urine, Saliva IC CN, SCN (138, 167) Medium- High CE SCN Blood High High 1-10 nL High High (33, 62, 63, 78, 79, 86, 124, 144-147, 150, 152, High Very High 1-10 μL Medium High High Blood, Urine, Saliva GC-NPD CN, SCN 155) (66, 70, 81, 140, 141, 151, 154, 156, 192) Very High Very High 1-10 μL High High High Blood, Urine, Saliva GC-ECD CN, SCN GC (45, 83, 94, 148, 153, 158) 1-10 μL High High Very High Extremely High Very High Blood, Urine, Saliva, Tissue CN, SCN, ATCA GC-MS a This table is meant to give a general overview of analytical techniques to analyze cyanide and its metabolites along with a general idea about parameters specifi c to each analysis technique. Parameters of specifi c methods within a particular analysis technique may be outside of those listed. b UV-Vis – ultraviolet visible spectrophotometry, AA – atomic absorption, LC – liquid chromatography, RP – reverse phase, MS-MS – tandem mass spectrometric detection, IC – ion chromatography, CE – capillary electrophoresis, GC – gas chromatography, NPD – nitrogen phosphorous detector, ECD – electron capture detector. c CN – cyanide, SCN – thiocyanate, ATCA – 2-amino-2-thiazoline-4-carboxylic acid. d These parameters are related to the general instrumental technique used and not each individual method of analysis.
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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
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Polymeric membrane based ion select
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Goal 2: Provide recommendations on
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hands-on training that develops a d
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Goal 3: Identify research needs to
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Working Group 1 Participants Bob KO
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estimated at roughly 3 to 5 days. H
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Goal 2 : Identify steps, agreements
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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 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: are many discrepancies in the liter
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
Page 130 and 131: The first three of these destructiv
Page 132 and 133: enforcement is minimal. There is an
Page 134 and 135: 1. Management/guidance to the Minis
Page 136 and 137: in Vietnam now and requires more ef
Page 138 and 139: Figure 2: Administrative structure
Page 140 and 141: References Baquero, J. (1999) Marin
Page 142 and 143: 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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