scholarly journals Metrological traceability of reference measurement procedures

2020 ◽  
pp. 6-12
Author(s):  
V. D. Sulaberidze ◽  
E. Skorniakova
Keyword(s):  
Metrological Traceability ◽  
Measurement Procedure ◽  
Practical Implementation ◽  
Measurement Standard ◽  
Reference Measurement ◽  
Measurement Result ◽  
Measurement Uniformity ◽  
Unit Of Measurement ◽  
A Chain ◽  
Continuous Chain

Metrological traceability is a key concept of measurement uniformity assurance, characterizing the property of a measurement result, according to which it can be correlated with a reference for comparison through a documented continuous chain of calibrations, each of which contributes to measurement uncertainty. A unit of measurement through its practical implementation, or a measurement technique that includes a unit of measurement for quantities other than ordinal, or a standard can serve as a basis for comparison. However, for many objects in biotechnology and medicine a system for confirming the correctness and required accuracy of the measurement result cannot be implemented. The paper discusses methods and schemes for the implementation of the principle of metrological traceability in the absence of a chain of metrological traceability of the measurement result to a measurement standard. A calibration hierarchy scheme is proposed that combines measurements based on reference measurement procedure and reference materials certified with their help, carried out in the chemical industry and medicine.

Proposal of a candidate international conventional reference measurement procedure for free thyroxine in serum

2007 ◽  
Vol 45 (7) ◽  
Author(s):  
International Federation of Clinica Thienpont ◽  
Graham Beastall ◽  
Nicholas D. Christofides ◽  
James D. Faix ◽  
Tamio Ieiri ◽  
...  
Keyword(s):  
Equilibrium Dialysis ◽  
Metrological Traceability ◽  
Measurement Procedure ◽  
Free Thyroxine ◽  
Tandem Ms ◽  
Reference Measurement ◽  
Reference Measurement Procedure ◽  
Liquid Chromatography Tandem Mass ◽  
Total Thyroxine ◽  
Lc Tandem Ms

AbstractIn the present paper the IFCC WG-STFT recommends and provides the rationale to establish metrological traceability of serum free thyroxine (FT4) measurements to a candidate international conventional reference measurement procedure. It is proposed that this procedure be based on equilibrium dialysis combined with determination of thyroxine in the dialysate with a trueness-based reference measurement procedure. The measurand is thus operationally defined as “thyroxine in the dialysate from equilibrium dialysis of serum prepared under defined conditions”. With regard to the trueness-based reference measurement procedure, the WG-STFT recommends use of an isotope dilution-liquid chromatography/tandem mass spectrometry (ID-LC/tandem MS) procedure for total thyroxine that has been optimized towards measurement at picomolar concentration levels and that is listed in the database of the Joint Committee for Traceability in Laboratory Medicine (JCTLM). For calibration, the purified thyroxine material IRMM-468 (resulting from a project funded by the European Commission and recently submitted to the JCTLM) is proposed. The WG-STFT stresses that according to this recommendation it is a prerequisite to strictly adhere to the defined equilibrium dialysis procedure, whereas it is permissible to introduce variants in the ID-LC/tandem MS procedure.Clin Chem Lab Med 2007;45:934–6.

scholarly journals Thrombin: An Approach to Developing a Higher-Order Reference Material and Reference Measurement Procedure for Substance Identity, Amount, and Biological Activities

2020 ◽  
Vol 125 ◽  
Author(s):  
Craig M. Jackson ◽  
M. Peter Esnouf ◽  
David L. Duewer
Keyword(s):  
Reference Material ◽  
Reference Materials ◽  
Biological Activities ◽  
Metrological Traceability ◽  
Catalytic Efficiency ◽  
Measurement Procedure ◽  
Protein Characterization ◽  
Reference Measurement ◽  
Reference Measurement Procedure ◽  
Hydrolytic Activities

Thrombin, the proteolytic enzyme that catalyzes the transformation of soluble fibrinogen to the polymerized fibrin clot, participates in multiple reactions in blood coagulation in addition to the clotting reaction. Although reference materials have existed for many years, structural characterization and measurement of biological activity have never been sufficient to permit claims of clear metrological traceability for the thrombin preparations. Our current state-of-the-art methods for protein characterization and determination of the catalytic properties of thrombin now make it practical to develop and characterize a metrologically acceptable reference material and reference measurement procedure for thrombin. Specifically, α-thrombin, the biologically produced protease formed during prothrombin activation, is readily available and has been extensively characterized. Dependences of thrombin proteolytic and peptide hydrolytic activities on a variety of substrates, pH, specific ions, and temperature are established, although variability remains for the kinetic parameters that describe thrombin enzymatic action. The roles of specific areas on the surface of the thrombin molecule (exosites) in substrate recognition and catalytic efficiency are described and characterized. It is opportune to develop reference materials of high metrological order and technical feasibility. In this article, we review the properties of α-thrombin important for its preparation and suggest an approach suitable for producing a reference material and a reference measurement procedure that is sensitive to thrombin’s catalytic competency on a variety of substrates.

scholarly journals Reference Measurement Procedure for Total Glycerides by Isotope Dilution GC-MS

2012 ◽  
Vol 58 (4) ◽  
pp. 768-776 ◽  
Author(s):  
Selvin H Edwards ◽  
Shelton L Stribling ◽  
Susan D Pyatt ◽  
Mary M Kimberly
Keyword(s):  
Isotope Dilution ◽  
Limit Of Detection ◽  
Metrological Traceability ◽  
Measurement Procedure ◽  
Chromotropic Acid ◽  
Serum Samples ◽  
Buffer Solution ◽  
Reference Measurement ◽  
Reference Measurement Procedure ◽  
The Mean

Abstract BACKGROUND The CDC's Lipid Standardization Program established the chromotropic acid (CA) reference measurement procedure (RMP) as the accuracy base for standardization and metrological traceability for triglyceride testing. The CA RMP has several disadvantages, including lack of ruggedness. It uses obsolete instrumentation and hazardous reagents. To overcome these problems the CDC developed an isotope dilution GC-MS (ID-GC-MS) RMP for total glycerides in serum. METHODS We diluted serum samples with Tris-HCl buffer solution and spiked 200-μL aliquots with [13C3]-glycerol. These samples were incubated and hydrolyzed under basic conditions. The samples were dried, derivatized with acetic anhydride and pyridine, extracted with ethyl acetate, and analyzed by ID-GC-MS. Linearity, imprecision, and accuracy were evaluated by analyzing calibrator solutions, 10 serum pools, and a standard reference material (SRM 1951b). RESULTS The calibration response was linear for the range of calibrator concentrations examined (0–1.24 mmol/L) with a slope and intercept of 0.717 (95% CI, 0.7123–0.7225) and 0.3122 (95% CI, 0.3096–0.3140), respectively. The limit of detection was 14.8 μmol/L. The mean %CV for the sample set (serum pools and SRM) was 1.2%. The mean %bias from NIST isotope dilution MS values for SRM 1951b was 0.7%. CONCLUSIONS This ID-GC-MS RMP has the specificity and ruggedness to accurately quantify total glycerides in the serum pools used in the CDC's Lipid Standardization Program and demonstrates sufficiently acceptable agreement with the NIST primary RMP for total glyceride measurement.

State of the Art in Trueness and Interlaboratory Harmonization for 10 Analytes in General Clinical Chemistry

2008 ◽  
Vol 132 (5) ◽  
pp. 838-846
Author(s):  
W. Greg Miller ◽  
Gary L. Myers ◽  
Edward R. Ashwood ◽  
Anthony A. Killeen ◽  
Edward Wang ◽  
...  
Keyword(s):  
Uric Acid ◽  
State Of The Art ◽  
Clinical Chemistry ◽  
Peer Groups ◽  
Measurement Procedure ◽  
Reference Systems ◽  
Reference Measurement ◽  
Clinical Laboratories ◽  
Routine Measurement ◽  
Fresh Frozen

Abstract Context.—Harmonization and standardization of results among different clinical laboratories is necessary for clinical practice guidelines to be established. Objective.—To evaluate the state of the art in measuring 10 routine chemistry analytes. Design.—A specimen prepared as off-the-clot pooled sera and 4 conventionally prepared specimens were sent to participants in the College of American Pathologists Chemistry Survey. Analyte concentrations were assigned by reference measurement procedures. Participants.—Approximately 6000 clinical laboratories. Results.—For glucose, iron, potassium, and uric acid, more than 87.5% of peer groups meet the desirable bias goals based on biologic variability criteria. The remaining 6 analytes had less than 52% of peer groups that met the desirable bias criteria. Conclusions.—Routine measurement procedures for some analytes had acceptable traceability to reference systems. Conventionally prepared proficiency testing specimens were not adequately commutable with a fresh frozen specimen to be used to evaluate trueness of methods compared with a reference measurement procedure.

scholarly journals Documenting metrological traceability as intended by ISO 15189:2012: A consensus statement about the practice of the implementation and auditing of this norm element

2019 ◽  
Vol 57 (4) ◽  
pp. 459-464 ◽  
Author(s):  
Marc Thelen ◽  
Florent Vanstapel ◽  
Pika Meško Brguljan ◽  
Bernard Gouget ◽  
Guilaine Boursier ◽  
...  
Keyword(s):  
Metrological Traceability ◽  
Measurement Procedure ◽  
Medical Laboratory ◽  
Clinical Samples ◽  
End User ◽  
Worst Case ◽  
Iso 15189 ◽  
Value Assignment ◽  
Traceability Chain ◽  
Medical Laboratories

Abstract ISO15189:2012 requires medical laboratories to document metrological traceability of their results. While the ISO17511:2003 standard on metrological traceability in laboratory medicine requires the use of the highest available level in the traceability chain, it recognizes that for many measurands there is no reference above the manufacturer’s selected measurement procedure and the manufacturer’s working calibrator. Some immunoassays, although they intend to measure the same quantity and may even refer to the same reference material, unfortunately produce different results because of differences in analytical selectivity as manufacturers select different epitopes and antibodies for the same analyte. In other cases, the cause is the use of reference materials, which are not commutable. The uncertainty associated with the result is another important aspect in metrological traceability implementation. As the measurement uncertainty on the clinical samples is influenced by the uncertainty of all steps higher in the traceability chain, laboratories should be provided with adequate and appropriate information on the uncertainty of the value assignment to the commercial calibrators that they use. Although the between-lot variation in value assignment will manifest itself as part of the long-term imprecision as estimated by the end-user, information on worst-case to be expected lot-lot variation has to be communicated to the end-user by the IVD provider. When laboratories use ancillary equipment that potentially could have a critical contribution to the reported results, such equipment needs verification of its proper calibration and criticality to the result uncertainty could be assessed by an approach based on risk analysis, which is a key element of ISO15189:2012 anyway. This paper discusses how the requirement for metrological traceability as stated in ISO15189 should be met by the medical laboratory and how this should be assessed by accreditation bodies.

scholarly journals Proposed Serum Cholesterol Reference Measurement Procedure by Gas Chromatography–Isotope Dilution Mass Spectrometry

2011 ◽  
Vol 57 (4) ◽  
pp. 614-622 ◽  
Author(s):  
Selvin H Edwards ◽  
Mary M Kimberly ◽  
Susan D Pyatt ◽  
Shelton L Stribling ◽  
Kara D Dobbin ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Gas Chromatography ◽  
Serum Cholesterol ◽  
Isotope Dilution ◽  
Isotope Dilution Mass Spectrometry ◽  
Measurement Procedure ◽  
Standard Reference Materials ◽  
Reference Measurement ◽  
Reference Measurement Procedure ◽  
The Mean

BACKGROUND Our purpose was to establish a mass spectrometry reference measurement procedure (RMP) for cholesterol to use in the CDC's standardization programs. We explored a gas chromatography–isotope dilution mass spectrometry (GC-IDMS) procedure using a multilevel standard calibration curve to quantify samples with varying cholesterol concentrations. METHODS We calibrated the mass spectrometry instrument by isotope dilution with a pure primary standard reference material and an isotopically enriched cholesterol analog as the internal standard (IS). We diluted the serum samples with Tris-HCl buffer (pH 7.4, 0.05 mol/L, 0.25% Triton X-100) before analysis. We used 17 serum pools, 10 native samples, and 2 standard reference materials (SRMs). We compared the GC-IDMS measurements with the CDC's modified Abell–Levy–Brodie–Kendall (AK) RMP measurements and assessed method accuracy by analyzing 2 SRMs. We evaluated the procedure for lack of interference by analyzing serum spiked with a mixture of 7 sterols. RESULTS The mean percent bias between the AK and the GC-IDMS RMP was 1.6% for all samples examined. The mean percent bias from NIST's RMP was 0.5% for the SRMs. The total %CVs for SRM 1951b levels I and II were 0.61 and 0.73%, respectively. We found that none of the sterols investigated interfered with the cholesterol measurement. CONCLUSIONS The low imprecision, linear response, lack of interferences, and acceptable bias vs the NIST primary RMP qualifies this procedure as an RMP for determining serum cholesterol. The CDC will adopt and implement this GC-IDMS procedure for cholesterol standardization.

Verification of Low-Density Lipoprotein Cholesterol Levels Measured by Anion-Exchange High-Performance Liquid Chromatography in Comparison with Beta Quantification Reference Measurement Procedure

2020 ◽  
Author(s):  
Daisuke Manita ◽  
Hiroshi Yoshida ◽  
Isao Koyama ◽  
Masakazu Nakamura ◽  
Yuji Hirowatari
Keyword(s):  
Anion Exchange ◽  
Clinical Laboratory ◽  
Measurement Procedure ◽  
Calculation Methods ◽  
Serum Samples ◽  
Cvd Risk ◽  
Blood Samples ◽  
Reference Measurement ◽  
Reference Measurement Procedure ◽  
Homogeneous Assays

Abstract Background A new lipoprotein testing method based on anion-exchange HPLC (AEX-HPLC) was recently established. We verified the accuracy of LDL-C levels, a primary therapeutic target for the prevention of cardiovascular disease (CVD), measured by AEX-HPLC comparing with LDL-C levels measured by beta quantification-reference measurement procedure (BQ-RMP), homogenous assays, and calculation methods. Methods We compared LDL-C levels measured by AEX-HPLC (adLDL-Ch: LDL-Ch and IDL-Ch) and BQ-RMP using blood samples from 52 volunteers. AdLDL-Ch levels were also compared with those measurements by homogeneous assays and calculation methods (Friedewald equation, Martin equation, and Sampson equation) using blood samples from 411 participants with dyslipidemia and/or type 2 diabetes. Results The precision and accuracy of adLDL-Ch were verified by BQ-RMP. The mean percentage bias [bias (%)] for LDL-C was 1.2%, and the correlation was y = 0.990x + 3.361 (r = 0.990). These results met the acceptable range of accuracy prescribed by the National Cholesterol Education Program. Additionally, adLDL-Ch levels were correlated with LDL-C levels measured by the 2 homogeneous assays (r > 0.967) and the calculation methods (r > 0.939), in serum samples from patients with hypertriglyceridemia. Conclusions AEX-HPLC is a reliable method for measuring LDL-C levels for CVD risk in daily clinical laboratory analyses.

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