바이오모니터링 프로그램을 위한 혈중 금속류 동시분석법 개발 및 확인 평가

차상원(Sangwon Cha),오은하(Eunha Oh),오세림(Selim Oh),한상범(Sang Beom Han),임호섭(Hosub Im) 한국환경보건학회 2021 한국환경보건학회지 Vol.47 No.1

Objective: Biological monitoring of trace elements in human blood samples has become an important indicator of the health environment. The purpose of this study was to detect and evaluate multiple metal items in blood samples based on ICP-MS, to perform comparative evaluation with the existing analysis method, and to develop and verify a new method. Methods: 100 µL of whole blood from 80 healthy subjects was used to analyze ten metals (Sb, tAs, Cd, Pb, Mn, Hg, Mo, Ni, Se, Tl) using ICP-MS. Verification of the analysis method included calculation of linearity, accuracy, precision and detection limits. In addition, a comparative test with the conventional graphite furnace atomic absorption spectroscopy (GF-AAS) method was performed. In the case of Pb, Cd, and Hg in whole blood, cross-analysis between Pb, Cd, and Hg analysis methods was performed to confirm the difference between the existing method and the new method (ICP-MS). Results: The coefficient of determination (R2 ) was 0.999 or higher in seven items and 0.995 or higher in three items. The Pb result showed that Pearson’s correlation coefficient was very high at 0.983, and the intraclass correlation coefficient was 0.966. The Cd result showed that Pearson s correlation coefficient was 0.917 between the existing method and the new analysis concentration value. Its intraclass correlation coefficient was 0.960, and there was no significant difference between the two groups. Hg had a low correlation at 0.687, and the intraclass correlation coefficient was 0.761, which was lower than that of Pb and Cd. The intra-day and inter-day accuracy of Pd and Cd were satisfactory, but Hg did not meet the criteria for both accuracy and precision when compared with the conventional analysis method. Conclusion: This study can be meaningful in that it proposes a more efficient and feasible analysis method by verifying a blood heavy metal concentration experiment using multiple simultaneous analyses. All samples were processed and analyzed using the new ICP-MS. It was confirmed that the agreement between the two methods was very high, with the agreement between the current and new methods being 0.769 to 0.998. This study proposes an efficient simultaneous methodology capable of analyzing multiple elements with small samples. In the future, studies of various applications and the reliability of ICP-MS analysis methods are required, and research on the verification of accurate, precise, and continuous analysis methods is required.

Original article : Simultaneous analysis and monitoring of thirteen preservatives in cosmetics by liquid chromatography

( Yong Jae Ryu ),( Gun Mook Yoon ),( Bang Han Yun ),( Bo Young Lee ),( Pil Ki Min ),( Ji Young Yun ),( Sang Yoon Nam ),( Beom Jun Lee ),( Young Won Yoon ) 한국예방수의학회 2013 예방수의학회지 Vol.37 No.2

The content of 13 preservatives was investigated for 107 sold in retail markets. A simultaneously analytical method of liquid chromatography, LC, for the preservatives in cosmetics was developed using an AvQuityTM Ultra performance LC System, Waters, BEH C18 column, 150mmx2.1mm,1.7 ㎛, and photo Diode Array, PDA, detector λ;220 nm for quantitative analysis, λ;190∼400nm for qualitative analysis. The developed instrumental method was validated using limit of detection, LOD, limit of quantification, LOQ, precision, accuracy, and linearity of standard curves. LOD and LOQ wre lower than 0.23mg/l and 0.75mg/l, respectively. When standard compounds were analyzed seven times consecutively at the LOQ level, precision and accuracy were lower than 2.49% and, 2.04%, respectively. Good linear relationships, R2 ⊇0.9998, were obtained for all compounds. Recoveries ranged between 96.03% and 102.61%and the overall variability was below 3%, RSD, The type of cosmetics showing the lowest detection rate of target compounds was sunscreen lotion, with a detection rate of 42.9%, followed by baby lotions and mask packs with the same detection rate at 69.2% At least one of the target preservatives was detected in 82.4% of creams, 93.3% of skin toners, 95.2% of lotions, and 92.9% of body lotions. Overall 79.4% of all samples contained at least one of the target compounds. The most frequently detected compound was phenoxyethanol. Methyl and propyl paraben also had a higher detection rate than the others, except, phenoxyethanol. Although the target preservatives in cosmetics sold in retail markets were detected by the simultaneous analysis of LC, the content of the detected preservatives was within the maximum allowed amount established by the Korean FDA.

HPLC-MS/MS를 이용한 벌꿀 중 동물용 의약품 동시분석방법 연구

김종화,문선애,김기유,정유정,이창희,구은정,윤미혜,이정복 한국식품위생안전성학회 2016 한국식품위생안전성학회지 Vol.31 No.2

This study was conducted to establish the simultaneous analysis method for veterinary drug residues in honey by high performance liquid chromatography tandem mass spectrometry (HPLC/MS/MS). The eleven targeting veterinary drugs with honey test method in Korean Food Standards Codex were divided into Group 1 (streptomycine dihydrostreptomycine, neomycine) and Group 2 (oxytetracycline, enrofloxacin, ciprofloxacin, cymiazole, chloramphenicol, amitraz, coumaphos, fluvalinate) to be analyzed simultaneously. From the results, the retention time(RT) of the targeting drugs was within 15 min, the range of detection limits was 0.0056 to 0.0643 μg/g and the range of quantification limits was 0.0169 to 0.1948 μg/g. The coefficients of determination(R2) for Group 1 (0.05~1.0 μg/mL) and Group 2 (0.01~1.0 μg/mL) were 0.9917~0.9987 and 0.9923~1.000 respectively, and showed the good linearity. The recovery rates for Group 1 (final conc. 0.25 μg/g) and Group 2(final conc. 1.0 μg/g) were 65.1~80.6% and 64.2~90.3% respectively. Also, the analysis results of inter day(n=3) and intra day(n=6) RSD(%) for area and retention time showed that the RSD(%) for area and retention time was below 10.92% and 1.57%. Therefore, the simultaneous analysis method of this study is evaluated to be a good test method for veterinary drug residues in honey.

산구절초, 자소엽, 찔레를 함유한 천연 화장품소재의다성분 동시분석과 항산화활성

함하늘,쉬레스타 아비나쉬 찬드라,김주은,이태범,유병완,김민숙,김광상,차준석,이용문,김종엽,임재윤 한국생약학회 2018 생약학회지 Vol.49 No.4

Recently, consumer demand for functional cosmetics containing natural ingredients has been greatly expanded. To develop the natural cosmetic materials, we selected 3 plants, Chrysanthemum zawadskii Herbich (CZ), Perilla frutescens (L.) Britton var. acuta Kudo (PF), and Rosa multiflora Thunberg (RM) which showed high total flavonoid contents (TFC), total polyphenol contents (TPC), and strong DPPH radical scavenging effect. We determined astragalin, chlorogenic acid, and rosmarinic acid as a marker compound for quantitative analysis of the content of each material and standardization of the quality standards and manufacturing standards through LC/MS analysis. HPLC-DAD was used to simultaneously analyze these marker components of three natural product complexes (Mix) and to validate the analytical method through experiments such as linearity, accuracy and precision. The detection wavelengths were set at 210, 265, and 330 nm. The detected 3 compounds from extract of CZ, PF, RM showed significant linearity (R2=0.9947). The limit of detection (LOD) of chlorogenic acid, astragalin and rosmarinic acid were 8.29 µg/ml, 2.28 µg/ml, and 27.00 µg/ml, respectively. The limit of quantification (LOQ) of chlorogenic acid, astragalin and rosmarinic acid were 25.11 µg/ml, 6.92 µg/ml, and 81.83 µg/ml, respectively. The contents of the three indicators of Mix were 19.82-24.71 mg/g of chlorogenic acid, 43.80-46.02 mg/g of astragalin, and 46.33-48.57 mg/g of rosmarinic acid.

Development of a simultaneous multiple solid-phase microextraction-single shot-gas chromatography/mass spectrometry method and application to aroma profile analysis of commercial coffee

Lee, C.,Lee, Y.,Lee, J.G.,Buglass, A.J. Elsevier 2013 Journal of chromatography A Vol.1295 No.-

A simultaneous multiple solid-phase microextraction-single shot-gas chromatography mass spectrometry (smSPME-ss-GC/MS) method has been developed for headspace analysis. Up to four fibers (50/30μm DVB/CAR/PDMS) were used simultaneously for the extraction of aroma components from the headspace of a single sample chamber in order to increase sensitivity of aroma extraction. To avoid peak broadening and to maximize resolution, a simple cryofocusing technique was adopted during sequential thermal desorption of multiple SPME fibers prior to a 'single shot' chromatographic run. The method was developed and validated on a model flavor mixture, containing 81 known pure components. With the conditions of 10min of incubation and 30min of extraction at 50<SUP>o</SUP>C, single, dual, triple and quadruple SPME extractions were compared. The increase in total peak area with increase in the number of fibers showed good linearity (R<SUP>2</SUP>=0.9917) and the mean precision was 12.0% (RSD) for the total peak sum, with quadruple simultaneous SPME extraction. Using a real sample such as commercial coffee granules, aroma profile analysis was conducted using single, dual, triple and quadruple SPME fibers. The increase in total peak intensity again showed good linearity with increase in the number of SPME fibers used (R<SUP>2</SUP>=0.9992) and the precision of quadruple SPME extraction was 9.9% (RSD) for the total peak sum.

동시 관계 유사 문법 항목 ‘-으며’, ‘-으면서’의 레지스터 분석 연구

백재파(Jae-Pa Baek) 동남어문학회 2022 동남어문논집 Vol.1 No.54

본 연구는 동시 관계 유사 문법 항목 ‘-으며’, ‘-으면서’의 레지스터 분포를 명확히 밝히는 데 있다. 이를 위해 세종코퍼스를 재구성하여 준거 코퍼스를 마련하였고, 구어/문어, 격식/비격식 구어 레지스터에 따른 분포를 분석하였다. 그리고 G2 값을 활용하여 분포 차이에 대한 통계적 유의성을 검증하였다. 분석 결과 ‘-으며’는 매우 구어적 문법 항목인 것으로 나타났으며(G2 2301.66), ‘-으면서’는 문어 레지스터에서 분포가 조금 더 많기는 하지만(G2 39.97) 구어 및 문어 레지스터에서 두루 사용되는 문법 항목인 것으로 분석되었다. 다음으로 격식 구어 레지스터에서의 분포를 분석한 결과 ‘-으며’와 ‘-으면서’ 모두 격식 구어 레지스터에서의 분포가 더 많은 것으로 나타났지만 ‘-으며’는 정도성이 약했으며(G2 29.47) ‘-으면서’는 통계적으로 유의미하지 않은 것으로 나타났다(G2 .95). 본 연구는 상반된 설명이 대립하는 유사 문법 항목에 대하여 객관적 결론을 도출하였고, 레지스터 분석 방법 및 기술 방안을 제시한 점에서 의의가 있다. This study aims to determine the distribution by register of the verbal suffixes -eumyo (-으며) and -eumyeonseo (-으면서) ‘while, during’ indicating simultaneous occurrence. To this end, a standard corpus was developed based on the Sejong corpus, and the distributions of the two forms by spoken/written and formal/informal speech registers were analyzed. The loglikelihood ratio (G2) values were then used to verify the statistical significance of the distributional differences. The results show that -eumyo is predominantly used in speaking (G2 = 2301.66), while -eumyeonseo is widely used in both spoken and written registers, though it is more common in the latter (G2 = 39.97). Both -eumyo and -eumyeonseo occurred more frequently in the formal speech register, although the difference was smaller for -eumyo (G2 = 29.47) than in writing, while the difference for -eumyeonseo was statistically insignificant (G2 = 0.95). This study allows objective conclusions to be drawn regarding similar grammatical items that have received conflicting explanations and is significant in showing the value of register analysis and depiction methods.

주택거래 증가의 경제적 파급효과 분석

변세일,황관석,박천규 국토연구원 2016 국토연구 Vol.88 No.-

This study aims to analyze the economic effects of increase in housing transactions using the simultaneous equations model and the input-output analysis. This study was conducted in two stages. First, we estimated the impact of increase in housing transactions on private consumption expenditure and residential building construction investment using the simultaneous equations model(K-MEM’14 model of KRIHS) and then used this result as a change of final demand for input-output analysis. Second, we analyzed the economic effect of increase in housing transactions in the real estate industries, related industries, and other industries using the input-output analysis. We can conclude that net growth of 153 thousands of housing transactions in 2013~2014 causes 2.234 trillion won in private consumption spending and 1.155 trillion won in residential building construction investment. And, these increase of final demand induces production of 6.65 trillion won, the value-added of 2.26 trillion won, the employment of 32.2 thousand people and wages of 1.15 trillion won. Finally, we could confirm that increase in housing transactions entirely contribute to national economy growth including real estate industry and related industry. 본 논문의 목적은 연립방정식 모형과 산업연관분석을 이용하여 주택거래의 경제적 파급효과를 분석하는 데 있다. 이를 위해 본 논문의 연구는 두 단계로 진행되었다. 먼저 최종수요의 변화를 추정하기 위해 연립방정식 모형인 국토연구원의 K-MEM’14 모형을 활용하여 주택거래 증가에 따른 민간소비지출 및 주거용 건물 건설투자 증가분을 추정하고 이를 투입산출 분석에서 최종수요의 증가분으로 활용하였다. 그다음으로 산업연관분석을 이용하여 부동산산업, 관련 산업, 기타 산업 등에 미치는 효과를 분석하였다. 분석 결과 2013~2014년 동안의 15만 3천 호 주택거래 증가는 민간소비지출 2조 2,340억 원, 주거용 건물 건설투자 1조 1,549억 원을 증가시키는 것으로 나타났다. 이러한 최종수요의 증가는 생산유발효과6조 6,466억 원, 부가가치 유발효과 2조 6,628억 원, 고용유발효과 3만 2,163.8명, 임금유발효과 1조 1,480억 원을 유발하는 것으로 분석되었다. 마지막으로 주택거래의 증가는 부동산산업과 관련 산업을 포함한 국민경제 전체 성장에 기여함을 확인할 수 있었다.

Allergen Sensitization Pattern by Sex: A Cluster Analysis in Korea

( Jungyoon Ohn ),( Seung Hwan Paik ),( Eun Jin Doh ),( Hyun-sun Park ),( Hyun-sun Yoon ),( Soyun Cho ) 대한피부과학회 2017 Annals of Dermatology Vol.29 No.6

Background: Allergens tend to sensitize simultaneously. Etiology of this phenomenon has been suggested to be allergen cross-reactivity or concurrent exposure. However, little is known about specific allergen sensitization patterns. Objective: To investigate the allergen sensitization characteristics according to gender. Methods: Multiple allergen simultaneous test (MAST) is widely used as a screening tool for detecting allergen sensitization in dermatologic clinics. We retrospectively reviewed the medical records of patients with MAST results between 2008 and 2014 in our Department of Dermatology. A cluster analysis was performed to elucidate the allergen-specific immunoglobulin (Ig)E cluster pattern. Results: The results of MAST (39 allergen-specific IgEs) from 4,360 cases were analyzed. By cluster analysis, 39 items were grouped into 8 clusters. Each cluster had characteristic features. When compared with female, the male group tended to be sensitized more frequently to all tested allergens, except for fungus allergens cluster. Conclusion: The cluster and comparative analysis results demonstrate that the allergen sensitization is clustered, manifesting allergen similarity or co-exposure. Only the fungus cluster allergens tend to sensitize female group more frequently than male group. (Ann Dermatol 29(6) 735∼741, 2017)

식육중의 잔류 항생.항균제의 검정에 관한 연구(III) Macrolide계 항생물질인 Erythromycin과 Tylosin의 Gas Chromatography/Mass Spectrometry 동시분석

류재천,송윤선,양종순,서지원,김명수,박종세 한국식품위생안전성학회 1993 한국식품위생안전성학회지 Vol.8 No.1

In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents n meat simultaneously, we studied a gas chromatogrphy-mass spectrometry (GC/MS) analysis. For a simultaneous analysis of macrolide antibiotics such as erythromycin and tylosin in meat, the homogenization with MeOH, defatting with n-hexane, extraction with CHCl3, elution with CHCl3 : MeOH=2:1 from Sep-Pak silica cartridge, acid gydrolysis, back extraction with CHCl3, and quantitation by selected ion monitoring(SIM) mode after trimethylsilyl derivatization were performed. The recoveries of erythromycin and tylosin (CV,%) at 10 ppm fortification level were 90.59(4.89) and 45.91(0.20) , and the detection limits of those were 0.02 and 2.0 $\mu\textrm{g}$/g beef, respectively. From these results, the developed analytical method using GC/MS-SIM mode allows excellent detection and quantitation of residual macrolide antibiotics in meats, using complementary method with bio-assay.

식육중의 잔류 항생.항균제의 검정에 관한 연구 (II) - Penicillin G , Chloramphenicol, Thiamphenicol, Gas chromatography/Mass spectrometry 동시 분석 -

류재천,양종순,서지원,김명수,박종세 한국식품위생안전성학회 1993 한국식품위생안전성학회지 Vol.8 No.1

어패류를 포함한 식용 육류중에 잔류하는 항생물질 및 항균성물질을 검출하기 위하여, 분석기기로서 Gas chromatography/ Mass spectrometry(GC/MS)를 사용한 동시분석법을 개발하였다. 여러 항생.항균제중에서 penicillin G, chloramphenicol, thiamphenicol을 중심으로 간단한 전처리과정과 유도체화를 하여 GC/MS 분석을 시행하였다. 전처리 과정을 요약하면 pH 4.0의 0.01 M EDTA-2Na McIlvaine buffer로의 추출, n-hexane으로의 탈지, Bond-Elute $C_{18}$ cartridge에 흡착된 물질의 0.01 M-methnolic oxalic acid로의 용출 그리고 건조 후 유도체화의 순으로 되어 있다. 본 방법에 의한 1 ppm spike시의 회수율은 penicillin G, chloramphenicol, thiamphenicol 각각 63.5%, 76.3%, 84.7%이었고, 검출한계는 각각 시료 g당 0.6, 0.085, $0.084\;\mu\textrm{g}$이었다. 또한 GC/MS 확인과정에서 실제 잔류농도가 1 ppm 이상이면 full scan spectrum으로 확인이 가능하였다. 이와 같은 GC/MS에 의한 잔류물질의 정량 및 확인시험은 앞의 미생물학적 방법의 복원은 물론 식품의 안전성 재고 및 규제독성의 측면에서도 매우 뜻 있는 연구라 하겠다. In an attempt to quantitate and qualitate residual antibiotics and antibacterial agents in meat simultaneously, we studied a gas chromatography-mass spectrometry(GC/M8) analysis. For a simultaneous analysis of penicillin G, chloramphenicol and thiamphenicol in meat, a simple and rapid clean-up procedure including extraction with 0.01 M EDTA-2Na Mcilvaine buffer (pH 4.0), defatting with n-hexane, and elution with 0.01M-methanolic oxalic acid from Bond Elute $C_{18}$ cartridge, and quantitation by selected ion monitoring (SIM) mode after derivatization was performed. The recoveries (%) of penicillin G, chloramphenicol and thiamphenicol (CV, %) at 1 ppm fortification level were 63.5 (7.6), 76.3 (8.1) and 84.7 (2.0), and the detection limits of those were 0.6, 0.085 and $0.084\;\mu\textrm{g}$ beef, respectively. This method using 81M mode allows excellent detection and quantitation of residual antibiotics and antibacterial agents in meat. Moreover, confirmation by a full scan electron impact mass spectrum is possible if residual level in the sample in above 1 ppm.