• Title/Summary/Keyword: Analytical Chromatography

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Biomonitoring of Toxic Effects of Pesticides in Occupationally Exposed Individuals

  • Arshad, Muhammad;Siddiqa, Maryam;Rashid, Saddaf;Hashmi, Imran;Awan, Muhammad Ali;Ali, Muhammad Arif
    • Safety and Health at Work
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    • v.7 no.2
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    • pp.156-160
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    • 2016
  • Background: Workers in pesticide manufacturing industries are constantly exposed to pesticides. Genetic biomonitoring provides an early identification of potential cancer and genetic diseases in exposed populations. The objectives of this biomonitoring study were to assess DNA damage through comet assay in blood samples collected from industry workers and compare these results with those of classical analytical techniques used for complete blood count analysis. Methods: Samples from controls (n = 20) and exposed workers (n = 38) from an industrial area in Multan, Pakistan, were subjected to various tests. Malathion residues in blood samples were measured by gas chromatography. Results: The exposed workers who were employed in the pesticide manufacturing industry for a longer period (i.e., 13-25 years) had significantly higher DNA tail length ($7.04{\mu}m$) than the controls ($0.94{\mu}m$). Workers in the exposed group also had higher white blood cell and red blood cell counts, and lower levels of mean corpuscular hemoglobin (MCH), MCH concentration, and mean corpuscular volume in comparison with normal levels for these parameters. Malathion was not detected in the control group. However, in the exposed group, 72% of whole blood samples had malathion with a mean value of 0.14 mg/L (range 0.01-0.31 mg/L). Conclusion: We found a strong correlation ($R^2=0.91$) between DNA damage in terms of tail length and malathion concentration in blood. Intensive efforts and trainings are thus required to build awareness about safety practices and to change industrial workers' attitude to prevent harmful environmental and anthropogenic effects.

Validation of HPLC Methods for Ascorbic Acid and Its Derivatives in Foods (식품 중 아스코르빈산 유래 산화방지제의 HPLC 분석법 검증 및 개선)

  • Jeong, Min Kyu;Park, Chan Uk;Park, Min Hee;Yeo, JuDong;Park, SeungKwan;Kim, SoHee;Shin, Tae-Sun;Baek, Hyung Hee;Lee, JaeHwan
    • Food Engineering Progress
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    • v.15 no.1
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    • pp.75-79
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    • 2011
  • Analytical methods for food antioxidants including ascorbic acid, erythorbic acid, ascorbyl palmitate (AP), and ascorbyl stearate (AS), were validated using high performance liquid chromatography. Validation parameters such as linearity, limit of detection (LOD), limit of quantification (LOQ), and recovery were tested using lard and cider as food model systems. Linearity of ascorbic acid and erythorbic acid were both higher than ($R^2$> 0.99), LOD of these compounds were 0.46 and 0.48 ${\mu}g/mL$, respectively and LOQ were 1.39 and 1.45 ${\mu}g/mL$, respectively. The recovery rates of these compounds were 86.35-94.78% and 84.76-95.02%, respectively. However, the concentration of AP and AS decreased in methanol stock solution. Four other solvents including ethanol, acetonitrile, mixture of methanol and acetonitrile, and mixture of ethanol and acetonitrile were tested to increase the stability of AP and AS under room temperature and refrigerated temperature. Ethanol provided better stability of AP and AS under both room and refrigerated temperature. This study can help to accurately analyze the content of ascorbic acid and its derivatives in processed foods.

Analytical Method of Multi-Preservatives in Cosmetics using High Performance Liquid Chromatography (HPLC 를 이용한 화장품 중 살균보존제 다성분 동시분석법 연구)

  • Min-Jeong, Lee;Seong-Soo, Kim;Yun-Jeong, Lee;Byeong-Chul, Lee
    • Journal of the Society of Cosmetic Scientists of Korea
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    • v.48 no.4
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    • pp.321-330
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    • 2022
  • This study attempted to establish an optimal multi-compound simultaneous analysis method that can secure reliable results for 15 - preservatives, 2 - sun screens and 1 - antioxidants of cosmetics using HPLC-PDA. Since the potential of hydrogen (pH) in the mobile phase affects the acid dissociation constant (pKa) of the preservatives, and the peak retention time shift and area change were observed. The peak separation condition was established by adjusting the pH to 0.1% H3PO4 addition (mL) when preparing the mobile phase. As a results of method validation, the linearity correlation coefficient (R2) of above 0.999 were obtained, and accuracy 87.9 ~ 101.1%, 0.1 ~ 7.6% precision for two types of cosmetics (cream and shampoo). It was found that the limit of detection (LOD) was 0.1 ~ 0.2 mg/kg and the limit of quantitation (LOQ) was 2.0 ~ 4.0 mg/kg. In addition, it was possible to simultaneously separate p-anisic acid, a natural compound that was difficult to separate in HPLC due to the small difference from methylparaben, a synthetic preservatives. Through this study, it will be effectively used to secure quality control and safety for compound that need restrictions on use cosmetics.

Phthalate Exposure Levels and Related Factors in the Urban Low-Income Group: Focus on a Residential Disadvantaged Community (도시 저소득층의 프탈레이트 노출수준과 관련 요인: 거주 취약집단을 중심으로)

  • Dahee, Han;Jiyun, Kang;Seohui, Han;Su Hyeon, Kim;Hohyun, Jin;Chahun, Kim;Hosub, Im;Ki-Tae, Kim;Yong Min, Cho
    • Journal of Environmental Health Sciences
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    • v.48 no.6
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    • pp.315-323
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    • 2022
  • Background: Socioeconomical disadvantaged communities are more vulnerable to environmental chemical exposure and associated health effects. However, there is limited information on chemical exposure among vulnerable populations in Korea. Objectives: This study investigated chemical exposure among underprivileged populations. We measured urinary metabolites of phthalates in urban disadvantaged communities and investigated their correlations with residential environment factors and relative socioeconomic vulnerability. Methods: Urine samples were collected from 64 residents in a disadvantaged community in Seoul. A total of eight phthalate metabolites were analyzed by liquid chromatography-mass spectroscopy. Analytical method used by the Korean National Environmental Health Survey (KoNEHS) was employed. Covariate variance analysis and general linear regression adjusted with age, sex and smoking were performed. Results: Several phthalate metabolites, namely monomethyl phthalate (MMP), monoethyl phthalate (MEP), mono-(2-ethyl-5-hydroxyhexyl) phthalate (MEHHP), and mono-n-butyl phthalate (MnBP) had higher levels than those reported in the adults of 4th KoNEHS. Notably, the MnBP level was higher in the lower socioeconomic group (geometric mean [GM]=47.3 ㎍/g creatinine) compared to non-recipients (GM=31.9 ㎍/g creatinine) and the national reference level (GM=22.0, 28.2 and 32.2 ㎍/g creatinine for adults, 60's and 70's, respectively.). When age, sex and smoking were adjusted, MEP and MnBP were significantly increased the lower socioeconomic group than non-recipients (p=0.014, p=0.023). The lower socioeconomic group's age of flooring were higher than non-recipients, not statistically significant. Conclusions: These results suggest that a relatively low income and aged flooring could be considered as risk factors for increased levels of phthalate metabolites in socioeconomic vulnerable populations.

Study Analysis of Isocycloseram and Its Metabolites in Agricultural Food Commodities

  • Ji Young Kim;Hyochin Kim;Su Jung Lee;Suji Lim;Gui Hyun Jang;Guiim Moon;Jung Mi Lee
    • Korean Journal of Environmental Agriculture
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    • v.42 no.1
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    • pp.71-81
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    • 2023
  • An accurate and easy-to-use analytical method for determining isocycloseram and its metabolites (SYN549431 and SYN548569) residue is necessary in various food matrixes. Additionally, this method should satisfy domestic and international guidelines (Ministry of Food and Drug Safety and Codex Alimentarius Commission CAC/GL 40). Liquid Chromatography-Tandem Mass Spectrometry (LC-MS/MS) was used to determine the isocycloseram and its metabolites residue in foods. To determine the residue and its metabolites, a sample was extracted with 20 mL of 0.1% formic acid in acetonitrile, 4 g magnesium sulfate anhydrous and 1 g sodium chloride and centrifuged (4,700 G, 10 min, 4℃). To remove the interferences and moisture, d-SPE cartridge was performed before LC-MS/MS analysis with C18 column. To verify the method, a total of five agricultural commodities (hulled rice, potato, soybean, mandarin, and red pepper) were used as a representative group. The matrix-matched calibration curves were confirmed with coefficients of determination (R2) ≥ 0.99 at a calibration range of 0.001-0.05 mg/kg. The limits of detection and quantification were 0.003 and 0.01 mg/kg, respectively. Mean average recoveries were 71.5-109.8% and precision was less than 10% for all five samples. In addition, inter-laboratory validation testing revealed that average recovery was 75.4-107.0% and the coefficient of variation (CV) was below 19.4%. The method is suitable for MFDS, CODEX, and EU guideline for residue analysis. Thus, this method can be useful for determining the residue in various food matrixes in routine analysis.

Persistence Study of Thiamethoxam and Its Metabolite in Kiwifruit for Establishment of Import Tolerance

  • Il Kyu Cho;Gyeong Hwan Lee;Woo Young Cho;Yun-Su Jeong;Danbi Kim;Kil Yong Kim;Gi-Woo Hyoung;Chul Hong Kim
    • Korean Journal of Environmental Agriculture
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    • v.41 no.4
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    • pp.355-364
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    • 2022
  • BACKGROUND: Pre-harvest interval and decline pattern of thiamethoxam were determined in kiwifruit using liquid chromatography-tandem mass spectrometry (LCMS/MS). The study was carried out to propose import tolerance using OECD maximum residue limit (MRL) calculator for the export promotion of kiwifruit to Taiwan. METHODS AND RESULTS: The thiamethoxam residue in kiwifruit was determined by using the LC-TriQ-MS/MS with the analytical process to set up the import tolerance under greenhouse conditions for Taiwan. Excellent linearity was observed for all of the analytes with a determination coefficient (R2)≥0.99. The limit of quantification was determined to be 0.01 mg/kg for both thiamethoxam and clothianidin in kiwifruit. Linearity was determined from the co-efficient of determinants (R2) obtained from the seven-point calibration curve. The standard calibration curve showed as follows; 1) Site 1 (Gimje): y = 944,406X + 1,583 (R2=0.9995), 2) Site 2 (Goheung): y = 1,356,205X + 934 (R2=0.9983), and 3) Site 3 (Jangheung): y = 1,239,937X - 3,090 (R2=0.9908). The residue of thiamethoxam in the kiwifruit for three decline trials showed the range of 0.35 to 0.56 mg/kg in site 1 (Gimje), 0.24 to 0.55 mg/kg in site 2 (Goheung), and 0.28 to 0.42 mg/kg in site 3 (Jangheung), respectively. However, clothianidin was not detected in all of the treatments. The maximum residual amounts (decline) in the samples, sprayed according to the safe-use standard for thiamethoxam 10% WG in kiwifruit (30 days before harvest, 3 sprays every 7 days) were 0.56 mg/kg in site 1, 0.55 mg/kg in site 2, and 0.42 mg/kg in site 3, respectively. CONCLUSION(S): The import tolerance (IT) of thiamethoxam for kiwifruit may be proposed to be 0.9 mg/kg by using the OECD MRL calculator.

Determination of Domoic Acid in Seafood Matrices using HPLC-UV with Solid Phase Extraction Cleanup (고체상 추출 전처리 및 HPLC-UV를 이용한 수산물 중 domoic acid의 분석)

  • Si Eun Kim;Sang Yoo Lee;Ji Eun Park;Hyunjin Jung;Hyang Sook Chun
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.297-304
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    • 2023
  • Domoic acid (DA), a neurotoxin produced naturally by diatoms, is responsible for incidents of amnesic shellfish poisoning. In this study, a modified analytical method was established to determine domoic acid in seafood using solid phase extraction cleanup and optimizing the amount of sample and extraction solvent to reduce interference effects. The modified method using high-performance liquid chromatography with ultraviolet detection was validated using three seafood matrices (mussel, red snow crab, and anchovy) at three concentrations (1, 2, and 4 mg/kg) and compared to the Food Code method. Compared to the Food Code method, the modified method showed better performance in terms of linearity (R2>0.999), detection limit (0.02-0.03 mg/kg), quantification limit (0.05-0.09 mg/kg), intra-/inter-day accuracy (86.2-100.4%), and intra-/inter-day precision (0.2-4.0%). Furthermore, the method was successfully applied for the analysis of 87 seafood samples marketed in Korea, and DA was detected at a low concentration of 140 ㎍/kg in one anchovy sample. These results suggest that the modified method can be used for routine determination of DA in seafood.

Monitoring Ochratoxin A in Coffee and Fruit Products in Korea (커피 및 과실류 가공품의 오크라톡신 A 모니터링)

  • Park, Ji-Eun;Heo, Seok;Lee, Mi-Seon;Kim, Eun-Jung;Park, Jong-Seok;Oh, Jae-Ho;Jang, Young-Mi;Kim, Mee-Hye
    • Korean Journal of Food Science and Technology
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    • v.42 no.3
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    • pp.263-268
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    • 2010
  • This research was conducted to evaluate the occurrence of ochratoxin A (OTA) in coffee and fruit products in Korea. A total of 388 coffee and fruit product samples were collected from retail or outlet markets; 177 samples were coffee and 211 were fruits or their products. Analytical methods including AOAC and Comit$\acute{e}$ Europ$\acute{e}$en de Normalisation (CEN) were selected and modified by method validation to detect and quantify the OTA in samples. All samples were analyzed by liquid chromatography with fluorescence detection. OTA was detected in 3.9% of 177 kinds of coffee and 0% of 211 kinds of fruit products. The levels of OTA were $0.7-4.6\;{\mu}g/kg$ in green coffee, $0.3-4.8\;{\mu}g/kg$ in roasted coffee, $1.4\;{\mu}g/kg$ in mixed coffee, and $0.4-0.6\;{\mu}g/kg$ in instant coffee. However, OTA was not detected in liquid coffee, dried fruits, or grape juice. OTA levels of all samples detected were less than the European Union legislation of $5.0\;{\mu}g/kg$ in coffee, $10.0\;{\mu}g/kg$ in raisins and $2.0\;{\mu}g/kg$ in grape juice. Therefore, the risk of OTA in coffee and fruit products in Korea is relatively low at safe levels.

Survey of Beet Red Contents in Foods using TLC, HPLC (TLC, HPLC를 이용한 식품 중 비트레드 함량조사)

  • Jang, Yaung-Mi;Lee, Tal-Soo;Hong, Ki-Hyoung;Park, Sung-Kwan;Park, Sung-Kug;Kwon, Yong-Kwan;Park, Jae-Seok;Chang, Sun-Young;Hwang, Hye-Shin;Kim, Eun-Jeong;Han, Yeun-Jeong;Kim, Byung-Sub;Won, Hye-Jin
    • Journal of Food Hygiene and Safety
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    • v.20 no.4
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    • pp.244-252
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    • 2005
  • This study was performed far development of new analytical method of beet red in foods. In this study, analysis of beet red in foods has been carried out by detection of betanine and isobetanine, the main color component of beet red as indicator compounds. The qualitative analysis technique consisted of clean-up of the colors with a $C_{18}$ cartridge, separation of the colors by cellulose TLC plate using acetone:3-methyl-1-butanol:distilled water (7:7:6) as a solvent system. Also, the quantitative analysis was performed using X-terra RP at wavelength 538 nm and $0.1\%$ phosphoric acid : methanol (90:10) as a solvent. The quantitative results of beet .ed were as follows:900.22$\∼$27701.60 $\mu$g/g for 60 item in nutrient supplement food, $21.95\∼713.40{\mu}g/g$ for 30 items and N.D. for 18 items in cindy, and $155.85{\∼}505.37{\mu}g/g$ for 12 items in ice creams, $43.52\∼64.75{\mu}g/g$ for 18 items and N.D. for 54 item in sauce, N.D. for 12 items in retort food.

Analysis of PAHs (polycyclic aromatic hydrocarbons) in Ground Coffee Using GC-tandem Mass Spectrometry and Estimation of Daily Dose (GC-tandem mass spectrometry를 이용한 분쇄원두커피 중 PAHs(polycyclic aromatic hydrocarbons) 분석법 연구 및 인체노출량 평가)

  • Jung, So-Young;Park, Ju-Sung;Son, Yeo-Joon;Choi, Su-Jeong;Lee, Yun-Jeong;Kim, Mi-Sun;Park, So-Hyun;Lee, Sang-Me;Chae, Young-Zoo
    • Korean Journal of Food Science and Technology
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    • v.43 no.5
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    • pp.544-552
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    • 2011
  • The purpose of this study was to develop an analytical method for determining 15 polycyclic aromatic hydrocarbons (PAHs) of EU priority using gas chromatography (GC)-tandem mass spectrometry (MS). The PAHs in ground coffee were analyzed after being extracted using methods such as saponification-liquid-liquid extraction, Soxhlet extraction, and solid-liquid extraction. The solid-liquid extraction method showed the greatest repeatability and most efficient reduction of the matrix effect. GC-tandem MS for the quantification of the 15 PAHs showed better resolution and lower limit of detections (LODs) than GC-MS-selected ion monitoring (SIM) and high performance liquid chromatography with fluorescence detector. LODs of this method for the ground coffee types were 0.002-0.1 ${\mu}g/kg$ and limit of quantifications (LOQs) were 0.006-0.2 ${\mu}g/kg$ The recoveries ranged from 52.6 to 93.3%. Forty-six commercial types of ground coffee were analyzed to determine their PAHs contamination levels. PAHs concentration ranged from ND to 5.988 ${\mu}g/kg$. This study was conducted with toxicity equivalence factors, the U.S. EPA recommendation to identify dietary risks for PAHs in different types of coffee. The estimated average daily dose of PAHs was $5.24{\times}10^{-8}$ mg/kg body weight/day.