• 한국축산식품학회지
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• 제36권3호
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• pp.319-325
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• 2016

This study was conducted to determine the residual amount of veterinary drugs such as meloxicam, flunixin, and tulathromycin in animal products (beef, pork, horsemeat, and milk). Veterinary drugs have been widely used in the rearing of livestock to prevent and treat diseases. A total of 152 samples were purchased from markets located in major Korean cities (Seoul, Busan, Incheon, Daegu, Daejeon, Gwangju, Ulsan and Jeju), including Jeju. Veterinary drugs were analyzed by liquid chromatography-tandem mass spectrometry according to the Korean Food Standards Code. The resulting data, which are located within 70-120% of recovery range and less than 20% of relative standard deviations, are in compliance with the criteria of CODEX. A total of five veterinary drugs were detected in 152 samples, giving a detection rate of approximately 3.3%; and no food source violated the guideline values. Our result indicated that most of the veterinary drug residues in animal products were below the maximum residue limits specified in Korea.

• 약학회지
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• 제57권5호
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• pp.330-336
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• 2013

"The Act on Medication Treatment of Sexual Impulse of Sex Offenders" known as chemical castration has been effective since July 2011 in Korea. According to the law, monitoring of male sex hormone in urine is enforced to request National Forensic Service more than once a month after injection of medicine designed to reduce sex impulse. We established a rapid and sensitive method for the monitoring of testosterone (T) and epitestosterone (E) in human urine by liquid chromatography with tandem mass spectrometry (LC-MS/MS). Three mL of urine was pretreated by solid-phase extraction for purification and performed enzymatic hydrolysis. The pretreated samples were extracted twice with 2 ml of ethyl acetate and n-hexane (2 : 3). The separation was applied on Thermo Hypersil GOLD C18 column ($1.9{\mu}m$, $100{\times}2.1mm$). A gradient elution of methanol and water of 0.1% formic acid were used as mobile phase and the retention time was less than 10 min. LC-MS/MS system coupled with an electrospray ionization source was performed in multiple reaction monitoring mode. The transitions of the analytes executed as following: m/z $289{\rightarrow}97$, 109 for T and E, m/z $292{\rightarrow}109$ for $T-d_3$ and $E-d_3$ as internal standards. The validation results of the method were satisfactory. The limits of detection were 0.05 ng/ml and the limits of quantification were 0.1 ng/ml. This method was successfully applied to real human urine sample. The developed method will be useful for monitoring T/E ratio in urine of sex offenders.

• 한국산업보건학회지
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• 제20권4호
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• pp.217-224
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• 2010

The purity methods to determine LOD/LOQ using standard deviation of the residual, intercept and blank by IUPAC and ACS describe many of the pitfalls and pose significant challenges to analytical chemists. Therefore, the aim of this study is the development of the simple, easy, convenient and statistically significant method to determine LOD in quantitative analysis of organic solvents by GC. The new approaching method by linearization in the given concentration range used coefficient of variation ; ${\sigma}_{n-1}$/S(standard deviation, ${\sigma}_{n-1}$ and average, S) of sensitivity(Response/concentration). The comparison of results among the purity methods(IUPAC and ACS) and the linearization have been fulfilled the F-test for standard deviations and t-test for LOD range values. The results of F-test and t-test are satisfied within 95 % confidence level, respectably. The LOD values determined by the new procedure are n-Hexane 0.0116 mg/$m^3$, Toluene 0.0807 mg/$m^3$, and o-Xylene 0.0494 mg/$m^3$. Because the standard deviation of the residual, intercept and blank and the slope of calibration curve are not calculated and the new approaching method use the coefficient of variation of sensitivity by linearization, this new method is simple, easy, convenient and statistically significant. In future, many chemical analysts will expect to applicate and routinely use this method in the all quantitative analysis.

• 한국약용작물학회지
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• 제24권4호
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• pp.271-276
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• 2016

Background: In the present study, we established an HPLC (high performance liquid chromatography)-analysis method for the determination of marker compounds as a part of the material standardization for the development of health-functional foods from Salvia plebeia R. Br. extract. Methods and Results: The quantitative determination method of hispidulin as a marker compound was optimized by HPLC analysis using a YMC hydrosphere C18 column with a gradient elution system. This method was validated using specificity, linearity, accuracy, and precision tests. It showed a high linearity in the calibration curve with a coefficient of correlation ($r^2$) of 0.999995. The method was fully validated, and was sensitive, with the limit of detection (LOD) at $0.09{\mu}g{\cdot}m{\ell}^{-1}$ and limit of quantification (LOQ) at $0.27{\mu}g{\cdot}m{\ell}^{-1}$. The relative standard deviation (RSD) values of the data from intra- and inter-day precision were 0.05 - 0.22% and 0.32 - 0.42%, respectively, and the intra- and inter-day accuracy of hispidulin were 99.5 - 102.3% and 98.8 - 101.5%, respectively. The average content of hispidulin in Salvia plebeia R. Br. extract was $3.945mg{\cdot}g^{-1}$ (0.39%). Conclusions: These results suggest that the developed HPLC method is very efficient, and that it could contribute to the quality control of Salvia plebeia R. Br. extracts as a functional ingredient in health functional foods.

• 한국환경농학회지
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• 제37권2호
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• pp.117-124
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• 2018

본 연구에서는 HPLC-UVD/MS를 이용하여 농산물 중 oxanthiin 살균제인 oxycarboxin의 잔류 분석법을 확립하였다. 대표 농산물은 현미, 콩, 배추, 고추 및 사과를 선정하였고 acetone을 가하여 추출된 oxycarboxin 성분을 dichloromethane 액-액 분배법과 Florisil 흡착크로마토그래피법으로 정제하여 HPLC-UVD/MS 분석대상 시료로 사용하였다. Oxycarboxin의 정량적 분석을 위한 최적 분석 조건을 확립하였으며, 정량한계(LOQ)는 0.04 mg/kg 이었다. 각 대표 농산물에 대해 정량한계, 정량한계의 10배 및 50배 수준에서 회수율을 검토한 결과 모든 처리농도에서 78.3~96.1% 수준을 나타내었으며, 반복 간 변이계수(CV)는 최대 4.7%를 나타내어 잔류분석 기준인 회수율 70~120% 및 분석오차 10% 이내를 충족시키는 만족한 결과를 도출하였으며, LC/MS SIM을 이용하여 실제 농산물 시료에 적용하여 재확인 하였다. 이상의 결과로 신규 oxycarboxin의 HPLC-UVD/MS 분석법은 검출한계, 회수율 및 분석오차 면에서 국제적 분석기준을 만족하는 신뢰성이 확보된 정량 분석법으로 사용 가능할 것이다.

• 환경위생공학
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• 제21권1호
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• pp.35-43
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• 2006

Formaldehyde is important because of their irritant and toxic properties, mutagenicity and carcinogenicity. In this study, liquid chromatography-mass spectrometry (LC-MS) is used for the analysis of formaldehyde after derivatization with 2,4-dinitrophenylhydrazine (DNPH) cartridge. Analytical parameters such as linearity, repeatability and minimum detection limit were evaluated. The linearity ($r^2$) was 0.9997 when analyte concentration ranges from 25 to $200{\mu}g/l$. The relative standard deviation (%RSD) was 1.25 % for concentration of $200{\mu}g/l$. The minimum detection limit (MDL) was 0.73 ppbv. It was shown that LC-MS method has a great potential for formaldehyde analysis. The results of formaldehyde from the survey of Ban-Woll and Shi-Hwa Industrial Complex samples, the highest level was 6.20, 3.93 ppb, respectively. The highest emission level of formaldehyde at chemical plants in the Ban-Woll' Shi-Hwa Industrial Complex was 5421.25 ppb.

• 한국결정성장학회지
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• 제21권6호
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• pp.274-279
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• 2011

연소 반응기를 이용하여 고분자 물질에 함유된 할로겐 원소인 브롬과 염소를 정량하기 위한 조건을 연구하였다. 염소농도 측정의 경우, Mohr법이나 전위차 적정법을 이용한 경우가 산-염기 적정법을 이용한 경우보다 분석 데이터 간 편차가 낮게 나타났다. 또한, 연소 반응기에서 단계별로 포집한 용액에 대한 염소와 브롬 측정 결과, 두 원소 모두 증류수를 흡수액으로 사용할 때, 0.3 M NaOH 수용액을 사용할 때보다 더 높은 회수율을 보였으며, 흡수액/세척액에서의 농도가 가스상의 형태로 배출되는 농도에 비해 높은 것으로 나타났다. 한편, 브롬 함량을 측정할 때, 연소 반응기를 이용한 경우가 XRF나 연소-이온크로마토그래피를 이용한 경우에 비해 농도가 상대적으로 낮게 평가되는 것으로 나타났다.

• 고문화
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• 66호
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• pp.87-112
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• 2005

Stain removal on ivory has been, for a long time, considered an undesirable treatment in conservation field because ivory is hygroscopic and anisotropic, having different physical properties in different directions. Cyclododecane, which sublimes at room temperature, has been investigated for its use in conservation field since 1995, as a reversible temporary consolidant, sealing agent or coating, water repellent, and barrier layer. This research aims to remove stains on ivory, temporarily protecting the none-stained area or painted area from methanol, acetone or the aqueous cleaning system using cyclododecane as a hydrophobic sealing agent. This research also aims to obtain information regarding whether cyclododecane can be safely and effectively used on archaeological wet ivory. Melted cyclododecane and saturated solutions of cyclododecane in mineral spirits, and hexanes were applied to ivory samples. Application methods, working properties of cyclododecane on ivory, and effect of cyclododecane coating on moisture content of wet ivory were evaluated. The sealing layer formed by molten cyclododecane or by saturated cyclododecane solution in hexane or saturated cyclododecane solution in mineral spirits did not form a secure contact with the surface of the highly polished ivory. The sealing formed with two different layers, in which saturated cyclododecane solution in hexane was applied initially and then molten cyclododecane was applied over the first layer, was found to securely protect the painted area. When the wet samples were kept in 100% RH environments for a month, active mold growths were observed except in the samples sealed with molten cyclododecane. In conclusion, cyclododecane was an efficient hydrophobic sealing agent to protect painting area while cleaning stains on ivory. It also prevented mold growing on wet ivory and wet bone. Evenness of cyclododecane film on ivory will be determined in UV light. Analytical techniques will include visual observation, polarized light microscopy, Scanning Electron Microscope, and Gas Chromatography.

• 한국환경보건학회지
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• 제36권2호
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• pp.155-162
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• 2010

Aflatoxin $B_1$, a known human carcinogen, is the member of aflatoxin subfamily that is most frequently found in contaminated foods. Epidemiological studies have suggested that aflatoxins may be associated with human liver cancer and acute hepatitis. Recently it was reported that the traditional medical herbs sold in domestic markets are contaminated with aflatoxins. Long-term administration of these contaminated medicines could result in adverse health effects. Therefore, it is important to evaluate the levels of exposure to aflatoxin in people who ingest traditional herbal medicines. Blood samples were collected, before and after the herbal medicine intake, from 151 subjects who visited the hospital. The metabolite of aflatoxin $B_1$ in blood, aflatoxin $B_1$-albumin (aflatoxin $B_1$-lysine), is reportedly an appropriate internal exposure indicator, and its levels in the collected bloods were therefore analyzed using a liquid chromatography-mass spectrometry. The analytical method of aflatoxin $B_1$-lysine in blood was firstly optimized in Korea and the levels were detected below quantification limits (2 pg/mg albumin) in this study population. Consequently, the exposure levels of aflatoxin $B_1$ by ingestion of herbal medicines were low but it is important to monitor routinely due to the possibility of risk on the aflatoxin exposure.

• 한국환경보건학회지
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• 제36권1호
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• pp.44-51
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• 2010

This study aimed to develop analytical method for 8-isoprostanes as biomarkers for oxidative stress with LC/MS/MS technique and to apply the method for human urine samples. Analyzed compounds for urinary oxidative stress markers were 7 stereo-isomers of prostaglandins and the internal standard (iso-$PGF_{2{\alpha}}-d_4$) was used to adjust the recovery rate. The method for determining urinary iso-$PGF_{2{\alpha}}$ consisted of solid phase extraction and LC/MS/MS detection. Separation of isomers of prostaglandins completed by porous graphitic carbon column and buffer solution. Detection limits for urinary markers of oxidative stress, iso-$PGF_{2{\alpha}}$ with LC/MS/MS were 0.01 ng/ml by S/N ratio 3 and 0.028 ng/ml by calculated as to FDA method. The recovery (92.8~101.9%) and precision (8.8~20.7%) of analysis were feasible for detecting iso-$PGF_{2{\alpha}}$ in real human urine samples. We detected 4 isomers of prostaglandins in human urine samples. Mean (standard deviation) of urinary iso-$PGF_{2{\alpha}}$ concentration were 0.231 (0.117) ng/mg creatinine for smoking group and 0.154 (0.082) ng/mg creatinine for non-smoking group.