Development of a Certified Reference Material from Caffeine Solution for Assuring the Quality of Food and Drug Measurements

Caffeine intake by pregnant women, adults and children can be harmful to the health of all particularly fetuses if the intake exceeds the permissible limits. Therefore, it is of fundamental importance to measure its concentration accurately using certified reference materials (CRMs). In the literature, no scientific details are published about the certification of caffeine standard solutions, and therefore, the present article covers this gap. A batch of caffeine solution was prepared in concentration of 1000 mg/kg and bottled. Homogeneity and stability of the candidate reference material were assessed by HPLC-UV and the results showed that the material is homogenous and stable enough. Characterization of the caffeine reference material was performed by HPLC-UV, LC-MS/MS and UV-VIS-NIR spectrophotometer in three different days and the characterization uncertainty was estimated in accordance with the requirements of ISO GUM. The certified value (999.86 ± 8.57 mg/kg) was derived as a weighted mean from the gravimetry and the three characterization methods and the certified uncertainty was calculated according to ISO Guide 35. The produced CRM is of strong interest to the food and drug analytical laboratories for the validity and credibility of their caffeine measurement results.

Certification of a Multicomponent Reference Material from Natural Gas Mixture by Gravimetry and Dual GC-FID/TCD System

Natural gas (NG) is one of the most important sources of energy for industrial and domestic consumption in the present era because it is cheap and free from sulfur impurities. Therefore, accurate and precise measurement of its composition is of fundamental importance for trade reasons. To improve the quality of NG gas measurements, certified reference materials (CRMs) should be used for calibration of measuring equipment in order to ensure the traceability of the measurement results to the SI units. For the traceability purpose, a multicomponent natural gas mixture was prepared gravimetrically as a reference material according to ISO 6142 from pure helium, hydrogen, n-pentane, i-pentane, n-butane, i-butane, propane, ethane, hexane, methane and nitrogen. The preparation was done in two dilution steps in 5 L aluminum cylinders. The calculated mole fractions and associated uncertainties of natural gas components were verified by a dual GC-FID/TCD system in accordance with ISO 6143 calibrated by a series of primary gas mixtures (CRMs) produced by an NMI. The results obtained by gravimetry and by GC measurements have been checked for compatibility as required by ISO 6142 and were found in very good agreement. Details of the preparation and calculation of the mole fractions and uncertainties of all gas components are explained in this article.

Development of a Certified Reference Material from Caffeine Solution for Assuring the Quality of Food and Drug Measurements

Caffeine intake by pregnant women, adults and children can be harmful to the health of all particularly fetuses if the intake exceeds the permissible limits. Therefore, it is of fundamental importance to measure its concentration accurately using certified reference materials (CRMs). In the literature, no scientific details are published about the certification of caffeine standard solutions, and therefore, the present article covers this gap. A batch of caffeine solution was prepared in concentration of 1000 mg/kg and bottled. Homogeneity and stability of the candidate reference material were assessed by HPLC-UV and the results showed that the material is homogenous and stable enough. Characterization of the caffeine reference material was performed by HPLC-UV, LC-MS/MS and UV-VIS-NIR spectrophotometer in three different days and the characterization uncertainty was estimated in accordance with the requirements of ISO GUM. The certified value (999.86 ± 8.57 mg/kg) was derived as a weighted mean from the gravimetry and the three characterization methods and the certified uncertainty was calculated according to ISO Guide 35. The produced CRM is of strong interest to the food and drug analytical laboratories for the validity and credibility of their caffeine measurement results.

CHOICE APPROACH OF THE OPTIMAL CERTIFICATION METHOD FOR CERTIFIED REFERENCE MATERIALS

将田口方法中代表设计研究或生产工艺研究中功能稳定性的信噪比概念用于标准物质定值方法的研究．为标准物质定值方法的优化提供数据处理模式和选择思路。以锌合金标准物质为例，采用原子吸收光谱法和紫外一可见分光光度法对锌合金标准物质中的铜元素定值，分别计算这两种方法定值数据的信噪比值，通过比较信噪比值的大小来判断两种分析方法的可靠性和分析体系的稳定性。

Accurate and precise determination of lead isotope composition in selected geochemical reference materials

Lead(Pb)isotopes have been extensively employed in tracing sources of Pb and its transport pathways through the environment.However,Pb isotopic ratios in related geochemical reference materials are scarce.Here,we report high-precision Pb isotopic ratios measured by Nu Plasma II MC-ICP-MS using calibrated ^(205)Tl/^(203)Tl=2.38865(NIST SRM 997)for mass discrimination correction.The long-term external precision(2SD)for NISTSRM 981 of Pb,BCR-2,and BHVO-2 are 0.31‰(n=105),0.42‰(n=11),and 0.25‰(n=5)for ^(208)Pb/ ^(206)Pb and 0.16‰,0.53‰,and 0.07‰for ^(206)Pb/ ^(207)Pb,both respectively,and their Pb isotopic ratios are in excellent agreement with the recommended values.Using this method,we report for the first time Pb isotopic compositions in shale SGR-1b(USGS);coal CLB-1(USGS);stream sediments GSD-17,-21,and-23(IGGE);soils GSS-12,-13,-14,-15,and-16(IGGE);plants GSV-1,-2,and-3(IGGE);and human hair GSH-1(IGGE).

Certification and uncertainty evaluation of flavonoids certified reference materials

Flavonoids are the most widely used in the field of the food, medicine, and cosmetic due to their pharmacological functions and biological activities, such as anti-tumor, anti-inflammatory and antioxidation. This work described the assignment of purity values to 3 flavonoids certified reference materials (CRMs) including baicalein, 5,7-dihydoxy flavones and naringenine which?were developed in this study according to the ISO Guides 34 and 35. The qualitative analysis was performed by liquid chromatography-mass spectrometry (LC-MS) and infrared spectroscopy (IR). The CRMs’ purity values were assigned based on the weighted average of quantitative nuclear magnetic resonance method and mass balance approach with high resolution liquid chromatography-VWD. All the three CRMs with following value mass fractions: baicalein at a certified purity P ± U (k = 2) of 98.8% ± 0.8%;5,7-dihydoxy flavones of 99.1% ± 0.7% and naringenine of 99.5% ± 1.0% respectively. The homogeneity of the CRMs was determined by an in-house validated liquid chromatographic method. Potential degradation during storage was also investigated and a shelf-life based on this value was established.

Determination of trace and rare-earth elements in Chinese soil and clay reference materials by ICP-MS

Inductively coupled plasma mass spectrometry(ICP-MS) has become a powerful tool for providing reliable analytical results in many laboratories around the word. In this study, the mixture of HF and HNO3 acids in high-temperature and high-pressure closed-vessel digestion technique were used to decompose some Chinese reference materials, and thirty seven elements were determined by ICP-MS. Most of the results for Chinese soil reference materials were found to be in reasonable agreement with the reference values, except Cs, Ta, Li, Ge, Zn, Nd, Tb and Ta whose values need to be revised. Their precisions were typically lower than 5% RSD. However, the Precisions of Chinese clay reference materials, especially for GBW03102 and GBW03102a, were significantly different with reference values, probably reflecting the existence of a coarser-grained fraction(>70 μm) in samples, and the formation of fluorides in Al-rich samples during sample decomposition by using the mixture of HF and HNO3 acids. Moreover, thirty-seven trace elements covering the mass range from Li to U in four Chinese clay reference materials were firstly provided with good precision and accuracy in this study.

Preparation and Certification of a New Salvianolic Acid A Reference Material for Food and Drug Research

Salvianolic acid A(Sal A),a water-soluble ingredient in Danshen,has various biological activities.Sal A and its impurities have similar physical and chemical properties,as well as strong reducibility;therefore,they are difficult to prepare and purify.In this study,high-purity Sal A was obtained by purification of sephadex chromatography and preparative chromatography.Furthermore,HPLC-DAD tandem ECD and HPLC-DAD tandem MS methods were used for non-volatile organic impurity analysis,ICP-MS method was used for non-volatile inorganic impurities and mass balance method and quantitative nuclear magnetic resonance were employed to certify the product.The structures of Sal A and its relative impurities were validated by nuclear magnetic resonance spectroscopy and mass spectrometry,and their contents were quantified as well.Following the principles of ISO Guides 34:2009 and 35:2005,a Sal A reference material was certified,covering homogeneity studies,stability studies,characterization,and uncertainty estimations.

PREPARATION AND CERTIFICATION OF THE HUMAN HAIR REFERENCE MATERIAL

The preparation of the human hair reference material and the steps taken to confirm its homogeneity and stability as well as its certificatipn are described. Certified values for 17 elements, which are of importance for human health, and reference values for the other 13 elements are provided for this material.

Preparation of bovine liver candidate reference material

The bovine liver candidate reference material specially for micro analytical techniques was prepared. The preparation process including material collection, dried, pulverize, sieve, homogenization and preliminary test was described in detail. The more effective grinding methods were established to achieve the median particle size of 22μm.

Scanning proton microprobe microanalysis for the assessmentof homogeneity of IAEA urban dust reference materials

In order to develop new reference materials for microanalytical nuclear techniques, scanning proton microprobe (SPM) technique was used to determine homogeneity level within 100×200 μm 2 micro area on the small pieces of IAEA urban dust reference materials. The experimental methods were described in detail. The results show that IAEA 396A/M Vienna urban dust is homogeneous enough for small sample analysis of standard reference material (SRM).

Determination of CeO_2 , Dy_2O_3, CuO and PbO in Yttrium Oxide Reference Material by Isotope Dilution Spark Source Mass Spectrometry

This paper describes the quantitative determination of rare-earth elements cerium, dysprosium and non-rare-earth element copper, lead and the homogeneity examination of these four elements in yttrium oxide reference material by isotope dilution spark source mass spectrometry (ID-SSMS). The sensitivity of the meth- od is l0^(-5)～10^(-7%). The precision is better than 6%. The accuracy is better than 5%. The interferences of the spectra and the optimum amount of the spike added to the sample are discussed. The choice of the conducting material for the sample electrodes is studied.

Titanium Isotope Analysis of Igneous Reference Materials using a Double-spike MC-ICP-MS Method

Ti separation was achieved by ion-exchange chromatography using Bio-Rad AG 1-X8 anion-exchange and DGA resins.For high-Fe/Ti and high-Mg/Ti igneous samples,a three-column procedure was required,whereas a two-column procedure was used for low-Fe/Ti and low-Mg/Ti igneous samples.The Ti isotopes were analysed by MC-ICP-MS,and instrumental mass bias was corrected using a ^(47)Ti-^(49)Ti double-spike technique.The ^(47)Ti-^(49)Ti double-spike and SRM 3162a were calibrated using SRM 979-Cr,certificated value ^(53)Cr/^(52)Crt rue=0.11339.Isobaric interference was evaluated by analysing Alfa-Ti doped with Na,Mg,Ca,and Mo,and results indicate that high concentrations of Na and Mg have no significant effect on Ti isotope analyses;however,Ca and Mo interferences lead to erroneousδ^(49/47)Ti values when Ca/Ti and Mo/Ti ratios exceed 0.01 and 0.1,respectively.Titanium isotopic compositions were determined for 12 igneous reference materials,BCR-2,BHVO-2,GBW07105,AGV-1,AGV-2,W-2,GBW07123,GBW07126,GBW07127,GBW07101,JP-1,and DTS-2b.Samples yieldδ^(49/47)Ti(‰)of−0.035±0.022,−0.038±0.031,0.031±0.022,0.059±0.038,0.044±0.037,0.000±0.015,0.154±0.044,−0.044±0.018,0.010±0.022,0.064±0.043,0.169±0.034,and−0.047±0.025(relative to OL-Ti,±2SD),respectively;of which isotopic compositions of DTS-2b,JP-1,GBW07101,GBW07105,GBW07123,GBW07126,and GBW07127 are reported for the first time.Standard Alfa-Ti was analysed repeatedly over a ten-month period,indicating a reproducibility of±0.047(2SD)forδ^(49/47)Ti,similar to the precisions obtained for geochemical reference materials.

Application of Coulometric Titration for the Certification of Primary Reference Materials of Pure Substances

In this article, the block scheme and metrological characteristics of the State primary standard of the mass (molar) fraction and mass (molar) concentration of the component in the liquid and solid substances and materials based on coulometric titration GET 176-2010 are given. Primary reference materials certified by coulometric titration in the Ural Scientific and Research Institute for Metrology include eight certified reference materials (CRMs) of pure solid substances (mostly salts of sodium or potassium) and one hydrochloric acid solution CRM. The metrological characteristics of these reference materials and the scheme of their application in titrimetric analysis are shown. The expanded uncertainty of the certified value (mass fraction for the solid substances or molar concentration for the solution) is in the range from 0.018% to 0.05%. Information about two primary reference materials of high purity iron and lead nitrate certified by controlled-potential coulometry with expanded uncertainty from 0.04% to 0.07% is also given.

REFERENCE MATERIALS

Potala PalaceConstruction of the Potala Palace began in the mid-7th century for the Tubo King Songtsan Gambo to greet his Han wife, Princess Wencheng. It comprised 999 rooms then, plus one built atop the Red Hill, which, said to have 1,000 rooms, was later destroyed by thunderbolts and wars. What we see today is a structure built during the 17th century.In the mid-17th century, the White House was added to the Potala Palace, which spread along the Red Hill in Lhasa.The palace is a structure of clay, wood and stone. The palace was the residence of the Dalai Lama of various generations. Beginning with the period of the 5th Dalai Lama, major religious and political ceremonies were held there.The palace covers a total area of 360,000 square meters, with major building rising 117 meters high in 13 floors, and extends some 360 meters from east to west.From 1989 to 1994, the State earmarked some 55 million Yuan and large quantities of gold and silver to repair the palace.In December 1994, the palace found its

Quality Assessment Statistic Evaluation of X-Ray Fluorescence via NIST and IAEA Standard Reference Materials

The aim of this study is a quality assessment of X-ray fluorescence laboratory located at the University of Khartoum. The X-ray fluorescence spectrometer system consists, a set of three 109Cd sources of an initial nominal activity of 10 μCi, and Si(Li) detector Energy Dispersive XRF(EDXRF) systems. It is important to carry out this work because it has an effective contribution for a wide range of research and services. The assessment was carried out by measuring 8 NIST-2709a (soil) and 13 IAEA-155 (milk powder) standard reference material samples for repeatability examinations to test the measurement precision. The total combined standards uncertainty values for XRF lab were estimated by an error from repeatability measurements adding 2.6% for error propagation related to the method. For accuracy assessment, three standard statistic approaches were applied, i.e. the Bias %, zeta-score, and En-number. The bias of all elements for both standard materials was found to be within a deviation range from −28% to 7.8%. The results of all elements for both the zeta-score test and En-number have satisfactory results except Th (Thorium) and Zr (Zirconium) which consider as questionable results for NIST SRM 2709a and unsatisfactory results for En-number.

Development of a certified reference material for visual inspection of unsound maize kernels

Maize unsound kernel content is one of the limited items in maize trade, and generally determined by sensory detection. A certified reference material(CRM) for visual inspection of maize unsound kernels was developed according to a national standard of China, GB 1353-2018, and five items, such as insect-damaged kernels, spotted kernels, broken kernels, sprouted kernels and moldy kernels, were included. Unsound maize kernels were collected from fields or prepared in a laboratory, then screened, and ten kernels demonstrating varying levels of unsoundness or damage for each item were embedded in epoxy resin. The CRM showed excellent homogeneity and stability, which was stable for 14 days at the temperature from-20℃ to 45℃ and for at least 18 months at room temperature out of direct sunlight and strong light. Co-laboratory confirmation showed the CRM conformed to the morphological characteristics described in GB 1353-2018. The research filled the gap of unsound maize kernel CRM in maize detection.

The Role of the American Oil Chemists’Society in World Trade——Quality Assurance Testing,Certified Reference Materials,and International Liaison Activities

The American Oil Chemists’ Society(AOCS) is a volunteer-led association. AOCS develops and publishes methods of analysis for fats, oils, proteins, surfactants, and related materials according to accepted international standards to ensure equitable trade practices on a global scale. AOCS Official Method development has been going on for over a hundred years. The founding vision of AOCS in 1909 was "an organization designed for the development and advancement of analytical methods for cottonseed products." AOCS Official Methods are essential to world trade and are used to confirm the value of billions of pounds of oilseed-based commodities and finished products each year. In addition, AOCS conducts proficiency testing, provides certified reference materials, and collaborates with other standards developers including the International Organization for Standardization(ISO) and the Codex Alimentarius Commission. AOCS serves as a professional scientific membership organization providing current and emerging information as well as disseminating research results in oils, fats, lipids, proteins, surfactants, and related materials. Several avenues are used, especially meetings, publications, interest groups, networking opportunities, and web presence. Many scientists, experts, and others engaged in working in these fields find their professional "home" in AOCS. The AOCS Technical Leadership Committee comprises some of the most experienced AOCS members and scientists. The AOCS Technical Services department staff relies on this committee for guidance on scientific matters and for advice in prioritizing the opportunities facing AOCS.

Preparation of Reference Material for Proficiency Test for Enumeration of Coliforms in Cheese Matrix

It is widely accepted that quantitative reference materials (RM), are indispensable tools for verification of the precision and accuracy of analytical measurements. The RM can be used by food microbiology laboratories, as part of their quality assurance programmes, to achieve their quality control. In Brazil, Anvisa RDC No. 12/01 specifies the enumeration of coliforms as one of the parameters for evaluating cheese quality. The aim of this study was to produce a quantitative RM for proficiency testing (PT) for use in the testing of enumeration of coliforms in cheese matrixes. A sample of an ultra-filtered cheese with a coliforms count of <3.0 MPN/g and a total n? of viable aerobes of 1.2 × 103 CFU/g was used as the matrix to produce the RM. The ultra-filtered cheese matrix was distributed in flasks, contaminated with a specific concentration of an Escherichia coli strain and submitted to freeze-drying. Sucrose was used as the cryo-protector. The RM produced was considered sufficiently homogeneous and stable at ≤ ?70?C during the entire study period (348 days). The material was also considered sufficiently stable at 4?C for six days, but instable at 30?C and 35?C for the same period. At ?20?C the RM was sufficiently stable for 161 days. It was concluded that the material showed all the necessary requirements for a quality RM to be used as PT items and could be transported to the laboratories taking part in a PT at up to 4?C for up to 6 days, since the results indicated maintenance of the cell concentrations during this period. This is the first study to describe a methodology for producing RM containing coliforms in a cheese matrix.