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A reliable measurement of blood folate levels is necessary in the clinical field to prevent serious diseases such as cognitive impairment and neural tube defects. Herein, the certification of the low-content folic acid (FA) and 5-methyltetrahydrofolate (5-Me-THF) in human plasma certified reference material (KRISS CRM 111-01-018) was performed. A human plasma pool obtained from the Korean Red Cross was used as a CRM candidate. The certification of the human plasma CRM was performed by isotope dilution ultra-performance liquid chromatography/tandem mass spectrometry. Two-dimensional liquid chromatography was employed to confirm the validity of the analytical method for FA due to the susceptibility of FA to matrix effects because of its limited quantity. The CRM stability was evaluated at -20 °C for 2 months and at -70 °C for up to 12 months to determine the certified value of the CRM. The certified value of the CRM was (84.6 ± 4.3) ng kg-1 and (5.80 ± 0.47) µg kg-1 for FA and 5-Me-THF, respectively. The homogeneity of the CRM was 1.64% and 3.10% for FA and 5-Me-THF, respectively. Further long-term stability assessments were conducted, indicating that the CRM remains valid for at least 58 months at -70 °C for FA and 48 months for 5-Me-THF. Compared to other blood-based CRMs, this CRM has lower folate levels, making it helpful in establishing analytical methods for a broader range of folate levels.

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Analytical methods based on the mass balance approach were developed for the purity evaluation of tetracycline hydrochloride, a representative salt compound used in pure veterinary drug analysis. The purity assignment method was used to quantify individual classes of impurities via independent analytical techniques. The mass fraction of the free base or salt form contained in a high-purity organic compound with a hydrochloride salt can be determined. The chloride content by ion chromatography-conductivity detector (IC-CD) and general classes of impurities, including structurally related impurities by liquid chromatography-ultraviolet (LC-UV) detector, water by Karl Fischer (KF) coulometric titration, residual solvents by headspace sampler gas chromatography/mass spectrometry (HS-GC/MS), and non-volatiles by thermogravimetric analyzer (TGA), were considered to calculate the purity of the mass fraction. The chloride content of the salt compound can be considered the main impurity in the mass fraction of the free base in the salt compound. A purity assay using quantitative nuclear magnetic resonance (q-NMR) as a direct determination method was performed to confirm the results of the mass balance method. The assigned purities of the tetracycline free form and its salt form in mass fraction were (898.80 ± 1.60) mg/g and (972.65 ± 1.58) mg/g, respectively, which are traceable to the international system of units (SI). Thus, the procedure for evaluating the purity of the free base and salt forms in the salt compound is newly demonstrated in this study.

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Phthalates are mainly used as plasticizers in polyvinyl chloride (PVC). However, prolonged exposure to phthalates poses considerable risks to human health. Consequently, the utilization of phthalates in consumer products is subject to regulations, with a defined threshold of 0.1 %. In this study, we developed an accurate and simultaneous method for determination of 11 representative phthalates and a non-phthalate plasticizer (di(2-ethylhexyl) terephthalate, DEHT) in PVC as a higher-order reference method. Homogeneously prepared PVC samples, each containing approximately 0.1 % of the target plasticizer compounds, were analyzed using gas chromatography-mass spectrometry (GC-MS) with deuterium-labeled phthalates and DEHT. The developed method could effectively separate and quantify all target plasticizers without interference with each other and potential overlap between the isomeric forms of phthalates, di-isodecyl phthalate, and di-isononyl phthalate. The developed method has high-order metrological quality, exhibiting exceptional selectivity, accuracy, repeatability (≤ 2.17 %), reproducibility (≤ 2.16 %), and relative expanded uncertainty (≤ 5.6 %). This analytical method is thus suitable for accurately assessing the target plasticizer levels in PVC products for ensuring compliance with the established 0.1 % threshold. This method was successfully applied to quantify twelve distinct plasticizers in PVC products obtained from the Korean market, validating its effectiveness and reliability in real-world scenarios.

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A certified reference material (CRM), KRISS CRM 108-02-006, was developed for the accurate analysis of low levels of acrylamide in infant formula matrices. The CRM is an infant formula fortified with acrylamide at a similar level as that stipulated by the European Union regulation for baby food. Commercially available infant formulas were processed by freeze-drying, and the subsequent homogenization of the fortified material to produce 961 bottles of the CRM in one batch. The CRM bottles containing approximately 15 g of the material in each unit were stored in a storage room at - 70 ℃. High-purity acrylamide was used as the primary reference material, and its purity was assessed using an in-house mass-balance method to obtain results metrologically traceable to the International System of Units. The acrylamide content of the infant formula CRM was evaluated using isotope dilution-liquid chromatography/mass spectrometry as a reference method, which was established by our research group. An acrylamide content of 55.7 ± 2.1 µg/kg was assigned as the certified value of the CRM with the expanded uncertainty at a 95% confidence level. The homogeneity study showed good uniformity of the acrylamide content among units, providing a relative standard deviation of 1.2% of the mean value. A stability study was also performed by monitoring the CRM under different temperature conditions and periods. The stability results indicated that the acrylamide content in the CRM under the storage conditions of - 70 ℃ remained stable for up to 10 months.

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A corn flour certified reference material (KRISS CRM 108-01-011) was developed to ensure accurate and reliable measurements of type B trichothecenes (deoxynivalenol, nivalenol, 3-acetyldeoxynivalenol, 15-acetyldeoxynivalenol), and deoxynivalenol-3-glucoside. The material was freeze-dried, ground, sieved, and well-mixed. The final produced CRM was packaged at 14 g per unit and stored at -70 °C. The certification was performed using isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS). For simultaneous characterization and homogeneity assessments, ten units were randomly selected and analyzed. The among-unit relative standard deviations were below 1 % for all mycotoxins, indicating excellent homogeneity of the CRM. The stability of the CRM was also assessed at various designated temperatures and test periods. The uncertainties of the certified values varied between 2.4 % and 6.2 %, thereby confirming their higher-order metrological quality to provide references for testing laboratories. In case of deoxynivalenol-3-glucoside, an information value was assigned due to the lack of its traceability to the SI units.

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An analytical method was developed for the accurate determination of eight polycyclic aromatic hydrocarbons (PAHs) in extruded high-impact polystyrene (HIPS) as a higher-order reference method. Uncleaned HIPS matrix rendered the accurate quantitation impossible and hampered the repeatability of the gas chromatography/mass spectrometry (GC/MS) measurement. This led to a bias in the results and increased the measurement uncertainty. Extracts were sufficiently purified through a two-step process: (i) dissolution and precipitation and (ii) molecularly imprinted polymers-solid phase extraction for clean-up. Co-elution of indeno(1,2,3-cd)pyrene (IP), dibenz(a,h)anthracene (DBahA), and their 13C6-labeled isotopes resulted in a bias in the area ratios of IP/13C6-IP and DBahA/13C6-DBahA, thus increasing the measurement uncertainty. An optimized GC condition using an Rxi-PAH column improved the peak separation of IP and DBahA and their isotopes, thus improving the quality of the measurement. The optimized method was validated using PAH (0.36-0.45 mg/kg)-containing HIPS pellets. The optimized method had excellent repeatability (<2%) and reproducibility (<3%) for concentrations less than 0.5 mg/kg of the eight PAHs in HIPS. Using the optimized method, the relative expanded uncertainties for all the target PAHs were below 5% (with a 95% level of confidence).

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We developed an isotope-dilution gas chromatography/high-resolution mass spectrometry (ID-GC/HRMS) method for the accurate determination of four polycyclic aromatic hydrocarbons (PAHs) in olive oil. The clean-up steps were optimized to sufficiently remove co-extracted oil matrix using the EZ-POP NP dual-layer and NH2 solid-phase extraction (SPE) cartridges. However, the cleaned sample still contained some matrix residues, which caused a bias. When 13C-labeled PAHs were used as the internal standards instead of deuterated PAHs, the recovery results improved in both low- and high-resolution MS conditions. Furthermore, the HRMS analysis facilitated to obtain more accurate results. The accuracy and precision of the optimized ID-GC/HRMS method were validated using PAH-fortified (0.5, 3, and 6 µg/kg) olive oil. The recoveries and relative standard deviations obtained for all the PAHs/levels were 97.5-102% and ~1%, respectively. Measurement uncertainties were generally within 5% (with a 95% confidence level).

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Infant formula certified reference material (CRM, KRISS CRM 108-02-003) were developed for the analysis of organic nutrients. The CRM is a milk-based infant formula powder, packaged at 14 g per unit. Ten thousand units were prepared and stored at -70 °C. For the certification of each nutrient, ten units were analyzed for simultaneous value-assignment and homogeneity test. Analytical methods used were isotope dilution mass spectrometry (IDMS) based on liquid chromatography mass spectrometer (LC/MS) or gas chromatography mass spectrometer (GC/MS) as higher-order reference methods.13 vitamins, 3 fatty acids, and total cholesterol were certified. The between-unit relative standard deviation of measurement results for each nutrient ranged 0.2% to 2.5%, showing very good homogeneity. The expanded relative uncertainties of the certified values ranged from 1% to 8%, indicating that they have higher-order metrological quality. The values of proximates (proteins, lipids, carbohydrates, water, and ash) were assigned through inter-laboratory comparisons.

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Herein, an isotope dilution-liquid chromatography-tandem mass spectrometry (ID-LC-MS/MS) method was developed as a candidate reference method for the accurate quantitation of hexabromocyclododecane (HBCDD) diastereomers in plastics. The repeatability, reproducibility, and uncertainty results showed that developed ID-LC/MS/MS method is reliable and reproducible. As homogeneous samples, HBCDD-containing extruded high-impact polystyrene (HIPS) pellets were fabricated via an extrusion process. Notably, we detected α-, ß-, γ-, δ-, ε-, η-, and θ-HBCDDs in the extruded HIPS pellets, and then determined their exact mass fractions using the ID-LC-MS/MS method. The relative contents (average ±â€¯standard deviation) of HBCDD diastereomers in HIPS obtained using the phenyl-hexyl column were 67.08 ±â€¯0.41% (α-HBCDD), 19.73 ±â€¯0.37% (ß-HBCDD), 11.59 ±â€¯0.16% (γ-HBCDD), and 1.6 ±â€¯0.07% (sum of δ-, ε-, η-, and θ-HBCDDs). These values differed significantly from the ones determined for the technical HBCDD mixtures (10.42% α-HBCDD, 5.30% ß-HBCDD, 82.13% γ-HBCDD, 2.15% minor HBCDDs) used to fabricate the HIPS pellets and thus demonstrating the HBCDD isomerization during the extrusion. The proportion of minor HBCDDs was smaller than the uncertainty of the total HBCDD and that the sum of α-, ß-, and γ-HBCDDs was comparable to the total HBCDD in the investigated samples. Notably, a real-life sample (expanded polystyrene board obtained from a local construction site) also showed a similar HBCDD profile, being rich in α-HBCDD.

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This study was performed to establish the proper liquid chromatographic conditions for the separation of hexabromocyclododecane (HBCD) diastereomers. Column selectivity towards HBCD diastereomers was evaluated for C18 and phenyl-hexyl stationary phases. First, the baseline separation of the primary HBCDs (α-, ß-, and γ-HBCD) was obtained using the ultra-performance liquid chromatography (UPLC) column with C18 stationary phase chosen in most previous studies for HBCD analysis; however, co-elution of δ- and ε-HBCD with the primary HBCD diastereomers was observed. To prevent the interference from δ- and ε-HBCD, we adopted a phenyl-hexyl UPLC column to resolve the HBCD diastereomers. The phenyl-hexyl UPLC column showed significantly different selectivity for the HBCD diastereomers compared with the C18 column, which allowed the clear isolation of δ-HBCD and ε-HBCD from the primary HBCD diastereomers. In addition, by checking the retention times of all HBCD diastereomers using both C18 and phenyl-hexyl columns, we confirmed the presence of δ-, ε-, η-, and θ-HBCDs in two technical HBCD mixtures.

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Patulin, a mycotoxin produced by several molds in fruits, has been frequently detected in apple products. Therefore, regulatory bodies have established recommended maximum permitted patulin concentrations for each type of apple product. Although several analytical methods have been adopted to determine patulin in food, quality control of patulin analysis is not easy, as reliable certified reference materials (CRMs) are not available. In this study, as a part of a project for developing CRMs for patulin analysis, we developed isotope dilution liquid chromatography-tandem mass spectrometry (ID-LC/MS/MS) as a higher-order reference method for the accurate value-assignment of CRMs. (13)C7-patulin was used as internal standard. Samples were extracted with ethyl acetate to improve recovery. For further sample cleanup with solid-phase extraction (SPE), the HLB SPE cartridge was chosen after comparing with several other types of SPE cartridges. High-performance liquid chromatography was performed on a multimode column for proper retention and separation of highly polar and water-soluble patulin from sample interferences. Sample extracts were analyzed by LC/MS/MS with electrospray ionization in negative ion mode with selected reaction monitoring of patulin and (13)C7-patulin at m/z 153→m/z 109 and m/z 160→m/z 115, respectively. The validity of the method was tested by measuring gravimetrically fortified samples of various apple products. In addition, the repeatability and the reproducibility of the method were tested to evaluate the performance of the method. The method was shown to provide accurate measurements in the 3-40 µg/kg range with a relative expanded uncertainty of around 1%.

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In 2009 and 2010, 720 serum samples were collected from non-occupationally exposed study participants at four Korean locations and monitored for the presence of 27 polybrominated diphenyl ether (PBDE) congeners. The median concentrations of Σ(27)PBDEs (the sum of 27 congeners) and Σ(3-7)PBDEs (the sum of tri- to hepta-BDE congeners) were 6.04 and 4.97 ng/g lipid, respectively. The most abundant congener detected in serum samples was BDE-153, followed by BDE-47 and BDE-99. The median value of Σ(3-7)PBDEs was similar to the median values observed in Asia and Europe, but much lower than that observed in North America. Some significant differences, based on geographic region and sex, were observed. We also observed a positive increase of BDE-153 with regard to age. In addition, we estimated the daily exposure to PBDEs from previously published reports of PBDE concentrations in food and dust, and determined the individual contributions of a variety of sources.

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An IRA-743 resin bulk sampler was validated to monitor long-term bulk deposition of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs). Six consecutive sampling campaigns (2008-2009) were conducted at four sites around steel complexes in Pohang, South Korea to investigate spatial and seasonal variations of PCDD/F bulk deposition. The bulk deposition within the steel complex showed the highest ∑(4-8)PCDD/F (Tetra-Octa) fluxes, ranging from 204 to 608 (mean: 352)pg m(-2)d(-1), indicating steel complexes were major sources of PCDD/Fs. The homologue profiles were dominated with lower chlorinated PCDFs. Furthermore, the prevailing winds were confirmed to influence the spatial distribution of PCDD/F deposition. There were apparent seasonal variations of the bulk deposition at each site, and seasonal homologue patterns of PCDD/Fs were clearly observed. According to the passive air sampling, however, no significant seasonal change of ambient air concentrations of PCDD/Fs was observed. Therefore, it was concluded that the seasonal variations of deposition fluxes of PCDD/Fs probably resulted from temperature-dependent gas/particle partitioning.

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XAD-2 resin based passive air samplers (PAS) were deployed for three one-year periods at the Korean polar and South Pacific research stations at Ny-Ålesund (2005-2009), King George Island (2005-2007), and Chuuk (2006-2009) to investigate long-range transport, local sources, and temporal trends of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs). The highest hexachlocyclohexane (HCH) concentration (35.2-78.9 pg·m(-3)) over the entire sampling period was detected at Ny-Ålesund, in the Arctic. α-HCH was the dominant OCP (31.1-67.1 pg·m(-3)), contributing about 50% of the total OCP load. Additionally, a high and consistent α/γ-HCH ratio was observed at Ny-Ålesund. HCHs might reach Arctic sites more easily than other OCPs from surrounding countries through long-range atmospheric transport (LRAT). Interestingly, high levels of the current-use OCP endosulfan-particularly endosulfan-I--were detected at almost all sampling sites, including in Antarctica, ranging 12.2-88.5, 17.7-130, and ND-59.7 pg·m(-3) at King George Island, Ny-Ålesund, and Chuuk, respectively. Specific OCP and PCB patterns, such as low trans/cis-chlordane ratios and a prevalence of lighter PCB congeners, were observed in all three regions (excepting one site at Ny-Ålesund and one site in the South Pacific affected by local sources) during all sampling periods. This indicates that these Polar and remote South Pacific sites are mainly influenced by LRAT. Over the entire sampling period, a decreasing trend of HCHs (α- and γ-HCH) and an increasing trend of endosulfan-I were observed at the Ny-Ålesund sites.

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A highly chlorinated flame retardant, Dechlorane Plus (DP), was measured in five fish species collected in 2008 from 22 river sites across South Korea. The sites consisted of 15 urban-industrial areas, three rural-industrial areas, and four rural rivers. Both syn- and anti-DP isomer were consistently detected in all fish samples regardless of sampling sites and fish species. DP has become a widespread environmental pollutant in South Korea. Concentrations of summation operatorDP isomers ranged from 0.61 to 126ngg(-1) lipid, with a mean concentration of 24.5ngg(-1) lipid. The mean summation operatorDP concentrations in the 15 urban sites (36.1+/-35.3ngg(-1) lipid) were approximately 25 times greater than those measured in the rural sites (1.4+/-1.0ngg(-1) lipid). The summation operatorDP concentrations in this study exceeded those determined in fish from the Great Lakes. DP exposure to fish is related to urbanization activity. Specific urban areas could be significant source areas of DP exposure, even in the absence of a local DP manufacturing facility. Concentrations of syn- and anti-DP isomer ranged from 0.17 to 30ngg(-1) lipid and 0.44 to 97ngg(-1) lipid, respectively. The anti-DP isomer was dominant in all samples. However, the mean f(anti) value for urban-industrial samples (0.67+/-0.060) was significantly lower than that of the technical DP standard (f(anti)=0.75; p=0.032). This observation supports that DP isomers exhibit different bioaccumulation behaviors and that syn-DP isomer more easily accumulates in biota samples than anti-DP isomer does.

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Four consecutive passive air samplings (September 2006-July 2007) were conducted at 15 sites around an iron and steel making plant in Pohang, Korea to investigate the spatial and seasonal distributions of polychlorinated biphenyls (PCBs) and ultimately the source-receptor relationships. Annual mean values of Sigma(8)PCBs (IUPAC number 8, 28, 52, 101, 118, 138, 153, 180) were in the range of 15.1-166 pg/m(3) with an average of 53.0 pg/m(3). The spatial distribution of PCBs for each sampling period clearly suggests that the steel complex is a major source of PCBs in this area, and the prevailing winds facilitated the atmospheric transport and dispersion of PCBs from the steel complex to the surrounding areas. Seasonal patterns of PCBs were observed clearly, which were influenced by meteorological conditions; the highest levels of PCBs were observed with the highest average air temperature, and the influence of rainfall (i.e., wet scavenging) was also observed. In addition, PCB 11, a non-Aroclor congener, was detected in high concentrations at all sites, implying that the sources of PCB 11 are both unique and ubiquitous. This study confirms that passive air sampling is a useful tool to obtain seasonal and spatial distributions of time-averaged POPs data at a local scale.

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Polychlorinated dibenzo-p-dioxins (PCDDs), polychlorinated dibenzofurans (PCDFs), and polychlorinated biphenyls (PCBs) in human have been studied extensively; however, polychlorinated naphthalenes (PCNs) have been studied less widely. The mean concentrations of PCNs, PCDDs, PCDFs, and PCBs in 61 healthy human volunteers were 2170 pg/g lipid, 452 pg/g lipid, 116 pg/g lipid, and 120 ng/g lipid respectively, and the mean toxic equivalents (TEQs) contributed by PCNs, PCDDs, PCDFs, and PCBs were 5.88, 5.22, 5.48, and 5.33 pg/g lipid, respectively. PCNs contributed to 26.8% of the total TEQs. 1,2,3,7,8-PeCDD, 2,3,4,7,8-PeCDF, PCB126, and hepta-CN-73 accounted for >62% of the total TEQs in the human serum samples. The overall serum PCN homologue profiles of all subjects were dominated by tetra- and penta-CN homologues, and the most predominant individual congener was hepta-CN-73, which contributed 17.5% of the total serum PCN concentration. Enrichment of hepta-CN-73 in the human serum samples might be due to contributors from combustion sources.

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To assess levels and seasonal trends of organochlorine pesticides (OCPs) and polychlorinated biphenyls (PCBs) in a high-altitude mountain region, a 2.1m snowpack sample was collected from the East Rongbuk Glacier at 6572 ma.s.l. on Mt. Everest in September 2005. This snowpack covered a full year period from the fall of 2004 to the summer of 2005 and reflected the major meteorology of the monsoon and non-monsoon seasons. The most abundant compounds detected in the snow samples were gamma-hexachlorocyclohexane (gamma-HCH) and alpha-HCH with mean concentrations of 123 pg L(-1) and 92 pg L(-1), respectively. This is the first detection of these compounds in recent snow samples from the Himalayas. Backward air trajectory analysis indicated that the Himalayas could be influenced by the major HCH source regions in both India and China. Among the seven marker PCB congeners (PCB 28, 52, 101, 118, 138, 153, and 180) quantified, PCB 28 and PCB 52 were the only dominant PCB congeners detected, with mean concentrations of 17 pg L(-1) and 6 pg L(-1), respectively. In addition, DDT metabolites, p,p'-DDE and p,p'-DDD were detected in some snow samples and mean concentrations of DDTs were 24 pg L(-1). Seasonal differences were observed for alpha- and gamma-HCH concentrations increasing from the non-monsoon season to the monsoon season. Meanwhile, PCB 28 and HCB showed uniform variations with peak concentrations resulting from an effective scavenging by snowfalls between the monsoon and non-monsoon interval. Compared to other high mountain areas, the levels of POPs deposited into the East Rongbuk Glacier were relatively low, resulting from the highest altitude and remoteness from source regions.

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To assess levels and patterns of polychlorinated biphenyls (PCBs) and organochlorine pesticides (OCPs) in polar regions, XAD-resin based passive air samplers were deployed for one year at the Korean polar research stations at Ny-Alesund, Norway (2005-2006) and King George Island, Antarctica (2004-2005). Backward trajectories suggest that these stations are affected by long-range transport from source regions in Northern Europe and Russia and the southern tip of South America, respectively. Relatively high levels of PCB-11, averaging 60 pg x m(-3), were observed in Antarctica, suggesting an unusual source of PCB-11 to the Southern Hemisphere. Reflecting the hemispheric distribution of global PCB emissions, the average level of sigma205PCB (excluding three mono-CBs and PCB-11) was five times higher in the Arctic (95 pg x m(-3)) than in the Antarctic (19 pg x m(-3)). Levels of sigma9PCB at Ny-Alesund were similarto those reported for other Arctic sites, while levels at King George Island were lower than at other sites on the Antarctic Peninsula but 1 order of magnitude higher than background levels measured at a more remote Antarctic site. Light homologues were predominant in all samples (except for one Arctic sample), consistent with the hypothesis of global fractionation and predictions of long-range transport potential. Dominance of heavy PCBs on the roof of the main building at Ny-Alesund and a concentration gradient with distance from the main building at King George Island strongly indicated the influence of local sources. OCP levels were also influenced by long-range transport but not by local sources. This study highlights the feasibility of using passive air sampling to assess both long-range transport and local pollution in remote regions.

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Coplanar polychlorinated biphenyls (PCBs), polychlorinated naphthalenes (PCNs), and polybrominated diphenyl ethers (PBDEs) were sampled using polyurethane foam (PUF) disk passive air samplers (PAS) at 19 sites in a heavily industrialized region of South Korea for 6 months (January-July 2006). The levels and spatial distribution of these three chemical groups were investigated to identify potential sources and transport in the study area, which can be divided into five regions: a steel-manufacturing complex, a residential area near the steel complex, a rural area, a semi-industrial area, and a petrochemical-manufacturing complex. Air concentrations (pg x m(-3)) were estimated using an average sampling rate of 3.0 m3 x day(-1) and ranged as follows: coplanar PCBs (0.8-16), PCNs (1.7-35), and PBDEs (3.8-24). The levels of coplanar PCBs and PBDEs were found to be the highest in the steel complex, followed by the petrochemical complex and the semi-industrial area. In addition, a high level of PCNs was measured near a petrochemical-processing plant. However, the residential area near the steel complex and the rural area showed relatively low concentrations of these chemicals, suggesting that the steel and petrochemical industries are probably important sources in the study area, but these potential sources do not strongly influence the surrounding areas.

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