Analysis of Natural Toxins by Liquid Chromatography-Chemiluminescence Nitrogen Detection and Application to the Preparation of Certified Reference Materials

2016 ◽  
Vol 99 (5) ◽  
pp. 1173-1184 ◽  
Author(s):  
Krista Thomas ◽  
Dominik Wechsler ◽  
Yi-Min Chen ◽  
Sheila Crain ◽  
Michael A Quilliam
Keyword(s):  
Reference Materials ◽  
Limit Of Detection ◽  
Certified Reference Materials ◽  
National Research Council ◽  
Complementary Method ◽  
Routine Monitoring ◽  
Wide Range ◽  
Measurement Results ◽  
Calibration Solution

Abstract The implementation of instrumental analytical methods such as LC-MS for routine monitoring of toxins requires the availability of accurate calibration standards. This is a challenge because many toxins are rare, expensive, dangerous to handle, and/or unstable, and simple gravimetric procedures are not reliable for establishing accurate concentrations in solution. NMR has served as one method of qualitative and quantitative characterization of toxin calibration solution Certified Reference Materials (CRMs). LC with chemiluminescence N detection (LC-CLND) was selected as a complementary method for comprehensive characterization of CRMs because it provides a molar response to N. Here we report on our investigation of LC-CLND as a method suitable for quantitative analysis of nitrogenous toxins. It was demonstrated that a wide range of toxins could be analyzed quantitatively by LC-CLND. Furthermore, equimolar responses among diverse structures were established and it was shown that a single high-purity standard such as caffeine could be used for instrument calibration. The limit of detection was approximately 0.6 ng N. Measurement of several of Canada's National Research Council toxin CRMs with caffeine as the calibrant showed precision averaging 2% RSD and accuracy ranging from 97 to 102%. Application of LC-CLND to the production of calibration solution CRMs and the establishment of traceability of measurement results are presented.

Development of reference materials with the composition of propyl and isopropyl alcohol solutions

2020 ◽  
pp. 66-72
Author(s):  
Irina A. Piterskikh ◽  
Svetlana V. Vikhrova ◽  
Nina G. Kovaleva ◽  
Tatyana O. Barynskaya
Keyword(s):  
Reference Materials ◽  
Measurement Errors ◽  
Isopropyl Alcohol ◽  
Certified Reference Materials ◽  
Toxic Substances ◽  
Biological Objects ◽  
Margin Of Error ◽  
Measurement Results ◽  
And Control ◽  
Characteristic Mass

Certified reference materials (CRM) composed of propyl (11383-2019) and isopropyl (11384-2019) alcohols solutions were created for validation of measurement procedures and control of measurement errors of measurement results of mass concentrations of toxic substances (alcohol) in biological objects (urine, blood) and water. Two ways of establishing the value of the certified characteristic – mass consentration of propanol-1 or propanol-2 have been studied. The results obtained by the preparation procedure and comparison with the standard are the same within the margin of error.

Arsenobetaine and other arsenic compounds in the National Research Council of Canada Certified Reference Materials DORM 1 and DORM 2

1998 ◽  
Vol 13 (3) ◽  
pp. 183-187 ◽  
Author(s):  
Walter Goessler ◽  
Doris Kuehnelt ◽  
Claudia Schlagenhaufen ◽  
Zdenka Slejkovec ◽  
Kurt J. Irgolic
Keyword(s):  
Reference Materials ◽  
Research Council ◽  
Certified Reference Materials ◽  
National Research Council ◽  
Arsenic Compounds

Development of Certified Reference Materials for Diarrhetic Shellfish Poisoning Toxins, Part 1: Calibration Solutions

2016 ◽  
Vol 99 (5) ◽  
pp. 1151-1162 ◽  
Author(s):  
Daniel G Beach ◽  
Sheila Crain ◽  
Nancy Lewis ◽  
Patricia LeBlanc ◽  
William R Hardstaff ◽  
...  
Keyword(s):  
Reference Materials ◽  
Large Scale ◽  
Certified Reference Materials ◽  
Shellfish Poisoning ◽  
Diarrhetic Shellfish Poisoning ◽  
Analytical Monitoring ◽  
Regulatory Testing ◽  
Standards And Guidelines ◽  
Calibration Solution ◽  
Planning Production

Abstract Okadaic acid (OA) and its analogs dinophysistoxins-1 (DTX1) and -2 (DTX2) are lipophilic polyethers produced by marine dinoflagellates. These toxins accumulate in shellfish and cause diarrhetic shellfish poisoning (DSP) in humans. Regulatory testing of shellfish is essential to safeguard public health and for international trade. Certified reference materials (CRMs) play a key role in analytical monitoring programs. This paper presents an overview of the interdisciplinary work that went into the planning, production, and certification of calibration-solution CRMs for OA, DTX1, and DTX2. OA and DTX1 were isolated from large-scale algal cultures and DTX2 from naturally contaminated mussels. Toxins were isolated by a combination of extraction and chromatographic steps with processes adapted to suit the source and concentration of each toxin. New 19-epi-DSP toxin analogs were identified as minor impurities. Once OA, DTX1, and DTX2 were established to be of suitable purity, solutions were prepared and dispensed into flame-sealed glass ampoules. Certification measurements were carried out using quantitative NMR spectroscopy and LC-tandem MS. Traceability of measurements was established through certified external standards of established purity. Uncertainties were assigned following standards and guidelines from the International Organization for Standardization, with components from the measurement, stability, and homogeneity studies being propagated into final combined uncertainties.

Certified Reference Materials and Metrological Traceability for Mycotoxin Analysis

2019 ◽  
Vol 102 (6) ◽  
pp. 1695-1707
Author(s):  
Zhen Guo ◽  
Xianjiang Li ◽  
Hongmei Li
Keyword(s):  
Reference Materials ◽  
Certified Reference Materials ◽  
Mutual Recognition ◽  
Metrological Traceability ◽  
International Standards ◽  
Great Effort ◽  
Legal Metrology ◽  
International Laboratory Accreditation Cooperation ◽  
Weights And Measures ◽  
Measurement Results

Abstract In the past decade, with the signing of the joint declaration by the International Bureau of Weights and Measures (BIPM), the International Organisation of Legal Metrology, the International Laboratory Accreditation Cooperation, and the International Organization for Standardization, and the issuing of new international standards such as ISO/IEC 17025 and ISO 13528, metrological traceability has become more and more important for the mutual recognition of measurement results. It is found that the important factors for ensuring the accuracy of results are not only relevant to calibrants but also to the analysis procedure. This paper focuses on the analysis of key factors that affect measurement results, such as analytical methods, reference materials (RMs), and proficiency testing of mycotoxins. The Capacity Building and Knowledge Transfer Programme for mycotoxins, led by the BIPM, which aims to establish a global measurement system traced to the Système International d’Unités (SI), is well illustrated. Furthermore, this paper suggests to stakeholders that great effort is needed to promote the effective use of certified RM resources that are traced to the SI and globally recognized by the International Committee for Weights and Measures to finally realize “one measurement, global recognition.”

scholarly journals Production of Certified Reference Materials for the Detection of Genetically Modified Organisms

2002 ◽  
Vol 85 (3) ◽  
pp. 775-779 ◽  
Author(s):  
Stefanie Trapmann ◽  
Heinz Schimmel ◽  
Gerard Nico Kramer ◽  
Guy van den Eede ◽  
Jean Pauwels
Keyword(s):  
Reference Materials ◽  
Genetically Modified Organisms ◽  
Production Control ◽  
Certified Reference Materials ◽  
Genetically Modified ◽  
Base Material ◽  
Genetically Modified Organism ◽  
International Organization ◽  
Roundup Ready

Abstract Certified reference materials (CRMs) are an essential tool in the quality assurance of analytical measurements. They are produced, certified, and used in accordance with relevant ISO (International Organization for Standardization) and BCR (Community Bureau of Reference) guidelines. The Institute for Reference Materials and Measurements (IRMM; Geel, Belgium) has produced the first powdery genetically modified organism (GMO) CRMs in cooperation with the Institute for Health and Consumer Protection (Ispra, Italy). Until now, different weight percentages in the range of 0–5%for 4 GMOs in Europe were produced and certified: Bt (Bacillus thuringiensis)-11 and Bt-176 maize, Roundup Ready® soybean, and MON810 maize. Bt-11 and Bt-176 maize and Roundup Ready soybean were produced by IRMM on behalf of Fluka Chemie AG (Buchs, Switzerland). Characterization of used base material is the first step in production and is especially important for GMO CRMs. The production of powdery GMO CRMs and methods used for production control are described. Thorough control of homogeneity and stability are essential for certification of reference materials and ensure validity of the certificate for each bottle of a batch throughout a defined shelf-life. Because production of reference materials and their maintenance are very labor- and cost-intensive tasks, the usefulness of new types of GMO CRMs must be estimated carefully.

scholarly journals A general strategy for the voltammetric trace determination of tellurium in geochemical and environmental matrices after arsenic coprecipitation and critical assessment of digestion schemes

2020 ◽  
Vol 17 (2) ◽  
pp. 85 ◽  
Author(s):  
Marc Biver ◽  
Montserrat Filella
Keyword(s):  
Reference Materials ◽  
Limit Of Detection ◽  
Chemical Elements ◽  
Certified Reference Materials ◽  
Anodic Stripping Voltammetry ◽  
General Strategy ◽  
Environmental Matrices ◽  
Hypophosphorous Acid ◽  
Sample Digestion

Environmental contextAmong chemical elements classified as elements of strategic importance, tellurium is rapidly becoming an emergent contaminant. There is, however, no accurate and sensitive method for measuring tellurium concentrations in environmental and geological samples (e.g., soils, sediments), and thus it is not possible to determine whether an ecosystem is being polluted by human activities. This study provides a reliable answer to this problem. AbstractA general method is proposed for the determination of tellurium in environmental and geochemical samples. Samples may be digested by any technique (acid or fusion digestion). The tellurium in the resulting solution is reductively coprecipitated with added arsenite by hypophosphorous acid, and the precipitate is redissolved and analysed by catalytic anodic stripping voltammetry. Several sample digestion techniques (acid and fusion digestions) are critically assessed. The method is applied to ore certified reference materials, with tellurium concentrations spanning three orders of magnitude, and sediment certified reference materials (ocean, lake and estuarine). An overall limit of detection (LOD) of 5 ppb is achieved. Acid digestion by H2SO4 and by HClO4 or sintering with Na2O2 in glassy carbon crucibles are shown to be the most adequate sample digestion techniques.

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