• Analytical Science and Technology
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• v.24 no.5
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• pp.352-359
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• 2011

An analytical method for solvent-free determination of benzene, toluene, ethylbenzene, and xylenes (BTEX) in water using repetitive membrane extractions coupled to cryofocusing and GC-MS was derived. BTEX compounds that permeated through a nonporous silicone membrane from the aqueous phase and evaporated into the acceptor phase were purged into a cryofocusing trap ($-100^{\circ}C$) with helium gas. The BTEX compounds, thus enriched in the trap, were thermally desorbed into a capillary column GC and detected using an MS. The flow rate of the donor phase (30 mL water) was set at 10 mL/min, and membrane extractions, accomplished by returning the water drained from the extraction module to the sample container, were repeated three times at $20{\pm}2^{\circ}C$. Although recoveries (%) were variable, from the highest for benzene (approximately 80%) to the lowest for ethylbenzene and xylenes (3.5-10%), the method showed satisfactory precision (RSD 2.2-10%) with good-linearity calibration curves ($r^2$ 0.9976-0.9997 in 1-100 ${\mu}g$/L range) for all of the compounds. The method detection limits (MDLs) ranged from 0.16 to 1.8 ${\mu}g$/L. The results showed the method's advantages such as short analysis time and overall simplicity without solvent compared to the conventional techniques.

• Journal of Food Hygiene and Safety
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• v.22 no.4
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• pp.257-267
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• 2007

The possibility of rapid non-destructive qualitative and quantitative analysis of vegetable oils such as perilla, com, soybean and rapaseed oils in sesame oils was evaluated. A calibration equation calculated by MPLS(Modified Partial Least Squares) regression technique was developed and coefficients of determination for perilla oil, com oil, soybean oil and rapaseed oil contents were 0.9992, 0.9694, 0.9795 and 0.9790 respectively. According to the data obtained from validation study, $R^2$ of contents of perilla, com, soybean, rapaseed oils were 0.997, 0.848, 0.957 and 0.968, and SEP of content of them 0.747, 5.069, 3.063 and 3.000 by MPLS respectively. The results indicate that the NIRS procedure can potentially be used as a non-destructive analysis method for the rapid and simple measurement of sesame oil mixed with other vegetable oils. The detection limits of the NIRS for perilla oil, com oil, soybean oil and rapaseed oil were presumed as 2%, $15{\sim}20%,\;15{\sim}20%$ and 10%, respectively.

• Journal of Food Hygiene and Safety
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• v.31 no.6
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• pp.432-438
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• 2016

Ethoxyquin (EQ, 1,2-dihydro-6-ethoxy-2,2,4-trimethyl-quinoline) is quinoline-based antioxidant used in the animal feed and food industry to protect the raw materials and final products against oxidation. In recent years the use of synthetic antioxidants in fishmeal ingredients carry-over to farmed fish fillets has received increasing attention in food safety. This study was conducted to develop an analytical method to determine EQ in aquatic products. The analytes were confirmed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). The sample was extracted with 1 N HCl (in case of flatfish extracted with 1 N HCl containing 10% acetonitrile). Then, solid phase extraction (SPE) was used for the cleanup. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.99, analyzed at 0.005-0.2 mg/kg concentration. The developed method was validated according to the Codex Alimentarius Commission (CAC) guideline. The limits of quantitation for EQ were 0.01 mg/kg. Average recoveries ranged from 81.3% to 107%. The repeatability of measurements, expressed as the coefficient of variation (CV, %), was below 10%. The analytical method was characterized with high accuracy and acceptable sensitivity to meet CODEX guideline requirements and would be applicable to analyze the EQ residue in aquatic products.

• Journal of Food Hygiene and Safety
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• v.32 no.3
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• pp.193-198
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• 2017

Scutellaria baicalensis, Eleutherococcus senticosus, and Angelica sinensis have been used as raw materials for health functional foods. This study was conducted to develop a novel method to analyze levels of baicalin (Scutellaria baicalensis), eleutheroside E (Eleutherococcus senticosus), and ligustilide (Angelica sinensis) simultaneously in health functional foods. The methanol extracted samples were analyzed and quantified via liquid chromatography-tandem mass spectrometry (LC-MS/MS) in the positive ion mode and the negative ion mode using multiple reaction monitoring. Standard calibration curves confirmed linearity with the correlation coefficient ($r^2$) of > 0.99 at $100-2000{\mu}g/mL$ concentration range. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of $13.0{\sim}35.2{\mu}g/L$ and $39.3{\sim}106.7{\mu}g/L$, respectively. The recovery results ranged between 91.4~109.9% at 3 different concentration levels with relative standard deviations (RSDs) less than 5%. The proposed analytical method was characterized with high accuracy and acceptable precision. The new method would be an effective tool to analyze baicalin, eleutheroside E, and ligustilide simultaneously in raw materials of health functional foods.

• Analytical Science and Technology
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• v.26 no.4
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• pp.221-227
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• 2013

A sensitive and selective liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the investigation of the ginsenoside Rg1 in human plasma. After addition of internal standard (digoxin), plasma was diluted with acetone and methanol (80:20), the supernatant was concentrated and analyzed by LC-MS/MS. The optimal chromatographic separation was achieved on an Agilent Eclipse XDB-C18 column ($4.6{\times}150mm$, $5{\mu}m$) with a mobile phase of 0.1% formic acid in water and 0.1% formic acid in methanol at a flow rate of 0.9 mL/min gradient mode. The standard calibration curve for ginsenoside Rg1 was linear ($r^2=0.9995$) over the concentration range 1~500 ng/mL in human plasma. The intra- and inter-day precision over the concentration range of ginsenoside Rg1 was lower than 7.53% (correlation of variance, CV), and accuracy exceeded 98.28%. This LC-MS/MS assay of ginsenoside Rg1 in human plasma is applicable for quantifying in the pharmacokinetic study.

• The Korean Journal of Pesticide Science
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• v.17 no.2
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• pp.107-116
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• 2013

Polar pesticides like pymetrozine (log $P_{ow}$: -0.18) are known to be difficult to analyze. The analytical method of pymetrozine using hydromatrix included in the official method of KFDA was uncommon and provided ambiguous evidence to confirm both the identity and the quantity. Therefore, precise single residue analytical method was developed in representative crops for using liquid-liquid extraction (LLE). The pymetrozine residue was extracted with methanol from 11 representative crops which comprised apple, blueberry, broccoli, cabbage, cherry, crown daisy, hulled rice, Korean cabbage, potato, rice and watermelon. The extract was purified serially by liquid-liquid extraction (LLE) and silica solid phase extraction (SPE). For rice and hulled rice samples, n-hexane partition was additionally adopted to remove nonpolar interferences, mainly lipids. The residue levels were analyzed by HPLC with DAD, using $C_8$ column. LOQ (limit of quantitation) of pymetroizinie was 1 ng (S/N > 10) and MQL (method quantitation limit) was 0.01 mg/kg. Mean recoveries from 11 crop samples fortified at three levels (MQL, 10 ${\times}$ MQL and 50 ${\times}$ MQL) in triplicate were in the range of 83.1~98.5% with coefficients of variation (CV) of less than 10%, regardless of sample type, which satisfies the criteria of KFDA. The method established in this study could be applied to most of crops as an official and general method for analysis of pymetrozine residue.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.42 no.1
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• pp.65-73
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• 2016

Korea Food and Drug Administration (KFDA) has officially announced 2,4-dinitrophenylhydrazine (DNPH) derivatization - high performance liquid chromatography (HPLC) methods for analysis of formaldehyde. This study was conducted to develop a convenient derivatization method for cosmetics by improving complex pre-treatment procedures included in KFDA method. To simplify pre-treatment procedures of KFDA method, reaction conditions including pH, time and temperature were optimized. This pre-treatment method does not require complicate pre-treatment steps of KFDA method such as pH adjustment of test solution with acetate buffer (pH 5.0), solvent-solvent partitioning with dichloromethane and concentrating procedure with vacuum evaporator. Formaldehyde-dinitrophenylhydrazone (formaldehyde-DNP) product produced by derivatization reaction was separated and quantified with a reversed-phase HPLC, which was slightly modified with KFDA method. The linearity test showed good results with 0.9999 of correlation coefficient ($r^2$) in the range of 2 ~ 40 ppm of standard solutions. In this method, limit of detection (LOD) and limit of quantitation (LOQ) values for formaldehyde were 0.2 ppm and 0.5 ppm, respectively. In addition, recovery test demonstrated that the method was also accurate and reproducible. Therefore, the proposed method can be applicable to rapid analysis of formaldehyde in cosmetics.

• Journal of the Korean Chemical Society
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• v.32 no.1
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• pp.37-47
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• 1988

The electrochemical behavior of 2-Amino-1-cyclopentene-1-dithiocarboxylate (acdc) was investigated by the use of polarography, cyclic voltammetry and cathodic stripping voltammetry at glassy carbon electrode. In this study, it was found that the dimer of the acdc was deposited on the glassy carbon electrode via one-electron oxidation process at +0.25V vs. SCE. The ring formation between two dithio group occurs along with the elimination of one sulfur atom. The elimination of sulfur atom occurs via two electron oxidation process at +0.8V vs. SCE. The most sensitive cathodic stripping peak due to the formation of the dimer was observed at -0.85V vs. SCE. The peak relationship between current and concentration was fairly linear in the range of 3${\times}10^{-5}{\sim}1.0{\times}10^{-6}$M. The preconcentration procedure enhanced the sensitivity about 100 times for the analysis of acdc using diffusion current. Detection limit was found to be $2.5{\times}10^{-7}$M and relative standard deviation was ${\pm}$4.1 % at $5.0{\times}10^{-6}$M DC polarography.

• Journal of the Korean Society of Food Science and Nutrition
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• v.42 no.2
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• pp.244-248
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• 2013

We studied the development of schizandrin as a marker compound in Jangsu Omija. Schizandrin was validated for its LOD (limit of detection), LOQ (limit of quantitation), precision, accuracy, and recovery by HPLC relative to Omija powder. It showed a high linearity in the calibration curve with a coefficient of correlation ($R^2$) of 0.9990. The LOD and LOQ were 0.2 ${\mu}g/mL$ and 0.5 ${\mu}g/mL$, respectively. The intra- and inter-day precision of schizandrin calibration standards was 0.06~0.66% and 0.13~1.19%, respectively, and the intra- and inter-day accuracy of schizandrin was 98.35~103.30% and 98.35~103.00%, respectively. Overall, schizandrin was validated through our analytical methods as a marker compound in Jangsu Omija.

• Journal of the Korean earth science society
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• v.26 no.7
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• pp.668-673
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• 2005

To collect or transfer samples of gaseous pollutants, various types of tubing are used. Hence, to analyze the uncertainties associated with the use of tubings, a series of comparative test were designed and conducted using the RSC standards with different concentration ranges. For the purpose of this study, we prepared tubings made of six different types of material which include: [1] silco-steel (S1), [2] stainless steel (S2), [3] silicone (S3), [4] PTFE Teflon (T1), [5] tygon (T2), and [6] brass (B). The patterns of RSC loss on to tubing walls, when compared on the basis of the least reactive material S1, exhibited that the extent of RSC loss varied dynamically. It was found that Teflon is highly stable. However, other materials tend to exhibit contrasting patterns of loss. S2 and B show significant loss of light RSC $(H_2S\;and\;CH_3SH)$, while S3 and T2 experience notable loss of heavy RSC (DMS and DMDS).