Twelve biological-matrix, agricultural/food reference materials, Corn Stalk (Zea Mays) (NIST RM 8412), Corn Kernel (Zea Mays) (NIST RM 8413), Bovine Musele Powder (NIST RM 8414), Whole Egg Powder (NIST RM 8415), Microcrystalline Cellulose (NIST RM 8416), Wheat Gluten (NIST RM 8418), Corn Starch (NIST RM 8432), Corn Bran (NIST RM 8433), Whole Milk Powder (NIST RM 8435), Durum Wheat Flour (NIST RM 8436), Hard Red Spring Wheat Flour (NIST RM 8437) and Soft Winter Wheat Flour (NIST RM 8438) were developed. They were characterized with respect to elemental composition via two extensive international interlaboratory characterization campaigns providing 303 reference and informational concentration values for 34 elements (Al, As, B, Ba, Br, Ca, Cd, Cl, Co, Cr, Cs, Cu, F, Fe, Hg, I, K, Mg, Mn, Mo, N, Na, Ni, P, Pb, Rb, S, Sb, Se, Sr, Ti, V, W, Zn) of nutritional, toxicological, and environmental significance. These products are available to the analytical community, for quality control of elemental composition analytical data, from the Standard Reference Materials Program, National Institute of Standards and Technology, Gaithersburg, MD, USA.
Authors:M. Mahajan, M. Prasad, H. Mhatre, R. Sawant, R. Rastogi, G. Rizvi, and N. Chaudhuri
A quartz pyrohydrolysis apparatus designed for the safe handling of pyrophoric carbide nuclear fuel samples while separating C1 and F trace impurities for quality control analysis is described. It has several advantages over the commonly used pyrohydrolysis apparatus. Performance of the apparatus during routine analysis of a large number of nuclear fuel samples has been found to be quite satisfactory.
Detailed results are presented in this paper for all analytical quality control samples distributed by the IAEA including
a new animal muscle intercomparison material of very low chromium content, and an attempt is made to draw some conclusions
regarding likely sources of analytical error.
The laboratory for INAA in Delft processes several thousands of samples per year for multielement determinations in a variety
of matrices. Samples are measured on different spectrometers (using well-type and coaxial detectors), by different persons
and using many different analytical protocols. All these results should be consistent with each other with respect to the
degree of accuracy, i.e., the combination of trueness and precision. A rigorous internal quality control program has been
implemented with automatic on-line evaluation. Annually an additional evaluation of the internal quality control results is
carried out using statistical techniques. The Naji-plot approach has proven to be an important graphical tool since it provides
direct insight in both trueness and precision. It is demonstrated that the degree of accuracy of the results obtained under
the large variety of operational parameters is under constant improvement.
The stems of Uncaria rhynchophylla (Miq.) ex Havil have a long history of use in traditional Chinese medicine to treat diseases and improve health. There is evident evidence that alkaloids constituents are mainly responsible for the beneficial effects of this plant medicine. The amounts of the major bioactive alkaloids in this plant vary widely with species, habitat, and as such, and establishment of a high-performance liquid chromatography (HPLC) fingerprint for quality control of this herbal medicine is of particular importance. The most alkaloids are used for medicine treatment and research. On the basis of the chromatographic data, a consistent HPLC fingerprint pattern containing 15 common peaks was obtained. Among these common peaks, four were identified as rhynchophylline, isorhynchophylline, corynoxeine, and isocorynoxeine. On the basis of this HPLC fingerprint and principal-components analysis, the quality of fifteen samples from different producing areas of China was objectively assessed. To summarize, the data described in this study offer valuable information for quality control and proper use of U. rhynchophylla (Miq.) ex Havil.
Authors:P. Vermaercke, P. Robouch, L. Sneyers, and F. De Corte
The thermal to epithermal neutron flux ratio (f) and the deviation of the epithermal neutron spectrum from the 1/E shape (α) are essential parameters for the correct application of k0-standardized neutron activation analysis. Several methods are applied for the determination of f and α. They are based on Cd-covered multi-monitor or on bare-irradiations methods. The recently developed and characterized synthetic
multi-element standards (SMELS) were designed as a validation tool for the proper implementation of the k0-NAA method in a laboratory. In particular, SMELS Type III contains Au and Zr, thus allowing the direct determination of f and α. It could, therefore, replace the traditional flux monitors. Furthermore, it could be used as a quality control material
to monitor the stability of the irradiation facility and the detector. This paper presents the accuracy of the f and α determination and the feasibility of quality control using SMELS for irradiation channel Y4 of the BR1 reactor.
Authors:S. Potamianos, A. Varvarigou, B. Costopoulos, N. Mitsokapas, and S. Archimandritis
Quality Control (QC) of radiopharmaceuticals is important, providing products of high standards. The current study refers
to an enzymic radioiodination method applied to the labeling of antibodies used in nuclear medicine and to the respective
QC procedures. Readily available materials such as125I, polyclonal immunoglobulin G (IgG) and a collection of simple chromatographic techniques helped establish a QC protocol
suitable for the radiochemical evaluation of radioiodinated biomolecules. A high pre-purification radiolabeling yield (90%)
for total protein was detected by paper electrophoresis (PE) and size exclusion chromatography (SEC), but only the inclusion
of SDS-PAGE confirmed the existence of “self-iodination” of lactoperoxidase (LPO) and revealed the true radiolabeling yield
Authors:K. Eigner Henke, M. Beran, J. Srank, and F. Melichar
The 90YCl3 radionuclide precursor (solution of 90Y3+ in diluted HCl) of high purity and high specific activity is already commercially produced and successfully used in nuclear
medicine. At the Nuclear Physics Institute ASCR, the 90YCl3 radionuclide precursor is prepared using extraction 90Sr/90Y generator (technology of centrifuge extractors with di-2-ethylhexylphosphoric acid, D2EHPA).1 Its radionuclidic, radiochemical, and chemical purity were examined and specified. The procedure developed for labeling of
DOTA-Tyr3-octreotide (DOTATOC) with carrier-free 86/90Y by Rösch2 at the Institute of Nuclear Chemistry of the University Mainz was optimized and modified in our Department of Radiopharmaceuticals
at NPI ASCR as standard labeling test (SLT) for analytical purposes. The SLT as a method for 90YCl3 radionuclide precursor quality control determining its labeling efficiency using ITLC SG chromatography is described and
proposed thereinafter. The labeling-efficiency of the tested batches of our product reached more than 95%.
Authors:E. Pączkowska, D. Smukowska, E. Tratkiewicz, and P. Białasiewicz
A simple and accurate reversed phase high-performance liquid chromatography (HPLC) method has been developed for the estimation of uniformity of dosage units, and delivered dose uniformity tests of fluticasone propionate and salmeterol xinafoate in samples obtained during the fine particle mass determination, using C8 Luna (2) 100A 100 × 4.6 mm, 5 micrometer particle size in gradient mode, with mobile phase comprising of buffer solution: 0.6% trifluoroacetic acid solution in water-tetrahydrofurane (8:2 v/v) and acetonitrile-methanol (1:1 v/v) in the ratio of 60:40 v/v. The flow rate was 1.5 mL min−1, and the detection was monitored by ultraviolet (UV) detector at 239 nm and 250 nm. Linearity was observed in the concentration range of 0.025–4.8 μg mL−1 for salmeterol xinafoate and 0.04–32.5 μg mL−1 for fluticasone propionate (R2 > 0.999). The recovery in the range from 98.2% to 102.7% and relative standard deviation (RSD) ≤ 2.2% demonstrated accuracy and high precision of the method. The quantification limit at an injection volume of 40 μL was 0.04 μg mL−1 for fluticasone propionate and 0.025 μg mL−1 for salmeterol xinafoate. The developed and validated method can be successfully applied for simultaneous quality control of dry powder inhalation products containing salmeterol xinafoate and fluticasone propionate in pharmaceutical industry.