• Analytical Science and Technology
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• v.23 no.6
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• pp.524-530
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• 2010

Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.

• Analytical Science and Technology
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• v.15 no.5
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• pp.417-426
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• 2002

Inductively Coupled Plasma Dynamic Reaction Cell Quadrupole Mass Spectrometry (ICP-DRC-QMS) was characterized for the detection of the six naturally occurring calcium isotopes. The effect of the operating conditions of the DRC system was studied to get the best signal-to-noise ratio. This experiment shows that the potentially interfering ions such as $Ar^+$, ${CO_2}^+$, ${NO_2}^+$, $CNO^+$ at the calcium masses m/z 40, 42, 43, 44 and 48 were removed by flowing $NH_3$ gas at the rate of 0.7 mL/min $NH_3$ as reactive cell gas in the DRC with a RPq value (rejection parameter) of 0.6. The limits of detection for $^{40}Ca$, $^{42}Ca$, $^{43}Ca$, $^{44}Ca$, and $^{48}Ca$ were 1, 29, 169, 34, and 15 pg/mL, respectively. This method was applied to the determination of calcium in synthetic food digest samples (CCQM-P13) provided by LGC for international comparison. The isotope dilution method was used for the determination of calcium in the samples. The uncertainty evaluation was performed according to the ISO/GUM and EURACHEM guidelines. The determined mean concentration and its expanded uncertainty of calcium was ($66.4{\pm}1.2$) mg/kg. In order to assess our method, two reference samples, Riverine Water reference sample (NRCC SLRS-3) and Trace Elements in Water reference sample (NIST SRM 1643d), were analyzed.

• Analytical Science and Technology
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• v.28 no.6
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• pp.460-466
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• 2015

An isotope dilution liquid chromatography tandem mass spectrometry was developed as a primary method for the quantitative analysis of cholesterol in infant formula. Cholesterol-d₄ was used as an internal standard and spiked into the infant formula sample. In order to release cholesterol out of cholesteryl ester, which is cholesterol bound to fatty acids in infant formula, saponification was carried out. Saponification conditions were optimized with heating temperature, reaction time and the concentration of KOH. The optimum conditions were as follows; heating temperature was 70 ℃, reaction time was 180 min and the concentration of KOH was 0.8 mL of 8 M KOH for about 0.1 g infant formula sample. Extraction of cholesterol out of sample solution was carried out with hexane uisng liquid-liquid extraction. Chromatographic analysis was carried out using Phenomenex Kinetex C₁₈ column. Mobile phase was 0.1% acetic acid in methanol/water (v/v, 99/1) and flow rate was 0.3 mL/min. Cholesterol and cholesterol-d₄ were monitored at mass transfer m/z 369/259 and 373/263 respectively. Reproducibility of the method was evaluated to be 0.23% of the measurement result. The expanded uncertainty of the measurement result of cholesterol in infant formula was approximately 1.9% at a 95% confidence level. NIST standard reference material having certified values of cholesterol in infant formula, was analyzed in order to verify this method. The ID-LC/MS/MS results were well agreed with the certified values of NIST SRM within the uncertainty.

• Analytical Science and Technology
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• v.21 no.6
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• pp.502-509
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• 2008

An ID LC/MS (isotope dilution liquid chromatography/mass spectrometry) was used as a primary method for the quantitative analysis of cholesterol in human serum. The separation of cholesterol was carried out by Thermo ODS hypersil $C^{18}$ column. The mobile phase was 100% methanol, and flow rate was $0.3m{\ell}/min$. Cholesterol and cholesterol-$3,4-13C_2$ were monitored at m/z 369.4 and 371.3, which correspond to $[M-H_2O+H]^+$ respectively. In order to verify the measurement method, NIST SRM 909b was analyzed. The results agreed well with certified values within uncertainty. The four kinds of serum certified reference material were prepared and certified. The repeatabilities of measurement were ranged from 0.1 to 0.8% (RSD), which were relatively good. The reproducibility between independent measurement run was below 0.24% (RSD). The expanded uncertainty was about 1.43% within the 95% confidence interval.

• Proceedings of the Korean Nuclear Society Conference
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• 1998.05b
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• pp.725-729
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• 1998

방사성 동위원소를 이용한 체외진단 측정법으로 RIA가 가장 널리 쓰여져 왔으나, 결합분획과 유리분획의 분리과정에서 오는 번거로운 단점을 개선하기 힘들었다. 1979년 Hart와 Greenwald에 의해 소개된 섬광근접측정법(Scintillation Proximity Assay, SPA)을 이용하여 RIA의 단점을 극복하고자 하는 연구가 시작되었다 주로 사용되는 방사성동위원소로 $^3$H, $^{125}$/I이 추천되는 핵종이며, 이 중에서 $^{125}$/I을 이용한 hCG(human chorionic gonadotropin) 체외진단법으로서 SPA의 기초연구를 수행하였다. SPA bead와 방사능 크기에 따라 측정되는 자연계수치의 증가와 hCG 표준물질을 농도별로 희석하여 유의성을 가지고 있는지 확인하였고, hCG 농도가 높은 것으로 판명된 환자의 혈청을 측정하여 임상적용의 가능성을 확인하였다.

• Analytical Science and Technology
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• v.16 no.4
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• pp.325-332
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• 2003

To analyze co-planar PCBs in food, the isotopic dilution method by high resolution gas chromatography/high resolution mass spectrometry was applied. Among 209 PCB congeners, 12 congeners (#77, #81, #126, #169, #105, #114, #118, #123, #156, #157, #167 and #189) were chosen as target compounds that were toxic congeners re-assessed by WHO in 1998. Milk and milk products including cheese and butter were collected as food samples. Samples were homogenized, spiked with the known amount of the standard mixture and extracted. After extraction, extracts were cleaned up by sulfuric acid impregnated silica gel, purified on silica gel and alumina column chromatography and then analyzed by HRGC/HRMS. As results, the overall recoveries were ranged from 83% to 106% and the limit of detection was about 0.1 pg/g at signal/noise>3. Levels of targets in the selected food samples were 0.001~0.107 pgWHO-TEQ/g.

• Analytical Science and Technology
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• v.14 no.4
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• pp.291-299
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• 2001

A method of separation and purification of Sm for quantitation of Sm isotopes from various fission products in PWR spent nuclear fuels has been studied. Simulated solution containing inactive metal ions(Cs, Ba, Gd, Eu, Sm and Nd) in place of radioactive fission products was prepared. Sm was separated with 0.5 M $HNO_3$/80% MeOH after washing with 1 M $HNO_3$/90% MeOH on AG $1{\times}8$, anion exchange resin. Sm was purified on cation exchange resin, AG $50W{\times}8$, pretreated with 0.2 M alpha-hydroxisobutyric acid(pH 4.5-4.6) to remove Ba causing isobaric effect Sm from PWR spent fuel. As a result of mass spectrometric measurement, eluted Sm portion did not include isobars form other elements such as Gd, Eu, Pm, Nd and BaO. The contents of Sm and its isotopes($^{147}Sm$, $^{148}Sm$, $^{149}Sm$, $^{150}Sm$, $^{151}Sm$, $^{152}Sm$ and $^{154}Sm$) in spent fuel were determined by isotope dilution mass spectrometric method spiking $^{154}Sm$.

• Analytical Science and Technology
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• v.14 no.5
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• pp.410-415
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• 2001

An analytical method has been developed which determines lead in steel samples by inductively coupled plasma mass spectrometry (ICP-MS) with sample introduction by the hydride generation. The lead hydride is not stable and requires and oxidant for the oxidation into metastable Pb(IV) before reduction to $PbH_4$ with $NaBH_4$. A study was carried out to find and optimum lead hydride generation condition for a sample solution with more than $1000{\mu}g/mL$ Fe matrix. $K_2Cr_2O_7$ was found to work as an efficient oxidant when more than $10{\mu}g/mL$ Fe matrix was present. Lactic acid was used with the oxidant as a complexing agent of the metastable Pb(IV) to enhance sensitivity. Optimum concentrations of the sample acidity, oxidant and lactic acid were different depending on the matrix concentration. The isotope dilution method was employed for the quantitation of lead. The determined Pb concentrations of the NIST steel SRM 361 and 362 were in good agreement with the certified values within the uncertainty range.

• Korean Journal of Organic Agriculture
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• v.21 no.3
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• pp.381-389
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• 2013

In order to study the effect of organic fertilizer on dry matter (DM) yield, nitrogen fixation and transfer from pea to barley, an experiment was carried out from May to June in 2008 in Incheon. A completely randomized block design with three replications was used for the experiment and one reference plot assigned each treatment for nitrogen fixation evaluation. Seeding mixture was 40kg barley and 80kg pea per ha. N rate of 40, 80 and 120kg/ha as organic fertilizer was applied at seeding. The equivalent of 1kg per ha as $(15NH_4)_2SO_4$ Solution at 99.8 atom N was applied to the plots ($30{\times}20cm$) at mid April. Forage was harvested from each plot in ripening stage at ground level and separated into barley and pea. Nitrogen fixation was 32.4%, 23.4% and 0% at three different organic N levels. Transfer rate were from 47.6% to 21.8% in difference method and 24.6% and 21.4% on $^{15}N$ dilution method. N Transfer amount were from 92.8kg/ha to 41.9kg/ha on difference method and 47.3kg in the 40kg N plots and 49.7kg in the 80kg N plots on $^{15}N$ dilution method but there was no N transfer in 120kg N organic fertilizer plots. Benefit from increased organic fertilizer was not clear in terms of nitrogen fixation and transfer from pea to barley in barley and pea mixtures.

• Analytical Science and Technology
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• v.18 no.4
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• pp.271-277
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• 2005

Urea in blood has been measured as an effective marker for diagnosis of renal function. Urea which is e end-product of nitrogen containing metabolites such as proteins is filtered through glomeruli of kidneys and then excreted as urine. If the renal function is deteriorated, the urea concentration in blood will be increased, from which the healthiness of renal function is judged. In order to improve the confidence of diagnosis results, the results must keep traceability chain to certified reference materials, which was certified by primary reference method. In this study, we proposed isotope dilution-liquid chromatography/mass spectrometry (ID-LC/MS) as a candidate primary method, in which $15^N_2$-urea is used as an internal reference material. The developed method is highly accurate in principle and is convenient as it does not require cumbersome derivatization. 0.1 mmol/L ammonium chloride was selected as a mobile phase for HPLC because it provided low interference in MS analysis of relatively low molecular weighted urea. HPLC and MS were connected with an electrospray ionization (ESI) interface of positive mode, which provided high sensitivity and reproducibility. The developed method was validated with internationally recognized reference materials, and we have obtained satisfactory results in an international ring trial. The expanded uncertainty calculated according to ISO guide was 1.8% at 95% confidence interval. The developed method is being used as a primary reference measurement method such as for certification of serum certified reference materials (CRMs).