• Title/Summary/Keyword: HPLC/FLD

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A Study on the Safety of Residual Pesticides in Cereal Grains and Pulses Agricultural Products Excluding Rice (잡곡 농산물의 잔류농약 안전성 조사)

  • Han, Na-Eun;Kim, Jae-Gwan;Yun, Hee-Jeong;Kang, Min-Seong;Cho, Young-Seon;Song, Ji-Won;Kim, Byeong-Tae;Lee, Seong-Nam;Choi, Ok-Kyung
    • Journal of Food Hygiene and Safety
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    • v.37 no.1
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    • pp.1-8
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    • 2022
  • In this study, the pesticide residues in 106 commercial cereal grains were monitored from February to July 2021. For the investigation, 40 domestic and 66 imported products from large, small-to-medium sized offline and online distribution channels, were collected and analyzed by using the multiresidue method for 341 pesticides on GC/ECD, GC/NPD, GC/MSMS, UPLC/PDA, HPLC/FLD, LC/MSMS. Pesticides were detected in total of 8 samples (7.5%), of which one was from big box retailers, two from small and medium-sized distribution stores, and five from online shopping mall. Five (4.7%) samples were found to have pesticide residues greater than the maximum residue limits (MRLs). The detected pesticides in kidney beans (1 case), mung beans (6 cases), and sorghum (1 case), were MGK-264, chlorpyrifos, thiamethoxam, malathion, piperonyl butoxide, and pirimiphos-methyl. Specifically, an excessive amount of thiamethoxam was found from the imported mung bean (5 cases).

Analysis of Pesticide Residues in Rice Straw for Livestock Feed (사료용 볏짚 중 잔류농약 분석)

  • Gil, Geun-Hwan;Kim, Jin-Bae;Kim, Chan-Sub;Son, Gyeong-Ae;Gwon, Hye-Yeong;Park, Jea-Eup;Lee, Kyu-Seung
    • The Korean Journal of Pesticide Science
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    • v.16 no.4
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    • pp.273-281
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    • 2012
  • This study was conducted for the establishment of the analytical method of pesticide residues in rice straw for 9 pesticides; etofenprox, tricyclazole, diazinon, edifenphos, propiconazole, carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran and for the monitoring of these pesticides in rice straw for livestock feed in Korea. These pesticides were classified into 4 groups according to analytical instrument condition. Group 1 (HPLC-UVD1) included tricyclazole and etofenprox while group 2 (HPLC-UVD2) included propiconazole and edifenphos. Group 3 (HPLC-FLD) included carbaryl, carbofuran, 3-hydroxy carbofuran and 3-keto carbofuran. Group 4 (GC-NPD) included Diazinon. The dried rice straw samples were extracted with acetone and purified by liquid-liquid partition and solid phase extraction (SPE): Combination of Florisil SPE and amino-propyl SPE was used for group 1 and group 2, amino-propyl SPE for group 3, and Florisil SPE was for group 4. Recovery was in the ranged 70~110% and the limits of quantitation (LOQ) were lower than the half of maximum residue limits. Therefore this method was proved to be efficient for monitoring of these pesticides residue in rice straw. A total of 18 rice straw samples from 6 provinces in Korea in 2010 were analyzed using established method and, only 3-keto carbofuran was detected in one sample at concentration of 0.04 mg/kg.

Vitamin B5 and B6 Contents in Fresh Materials and after Parboiling Treatment in Harvested Vegetables (채소류의 수확 후 원재료 및 데침 처리에 의한 비타민 B5 및 B6 함량 변화)

  • Kim, Gi-Ppeum;Ahn, Kyung-Geun;Kim, Gyeong-Ha;Hwang, Young-Sun;Kang, In-Kyu;Choi, Youngmin;Kim, Haeng-Ran;Choung, Myoung-Gun
    • Horticultural Science & Technology
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    • v.34 no.1
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    • pp.172-182
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    • 2016
  • This study was aimed to determine the changes in vitamin $B_5$ and $B_6$ contents compared to fresh materials after parboiling treatment of the main vegetables consumed in Korea. The specificity of accuracy and precision for vitamin $B_5$ and $B_6$ analysis method were validated using high-performance liquid chromatography (HPLC). The recovery rate of standard reference material (SRM) was excellent, and all analysis was under the control line based on the quality control chart for vitamin $B_5$ and $B_6$. The Z-score for vitamin $B_6$ in food analysis performance assessment scheme (FAPAS) proficiency test was -1.0, confirming reliability of analytical performance. The vitamin $B_5$ and $B_6$ contents in a total of 39 fresh materials and parboiled samples were analyzed. The contents of vitamin $B_5$ and $B_6$ ranged from 0.000 to 2.462 and from 0.000 to $0.127mg{\cdot}100g^{-1}$, respectively. The highest contents of vitamin $B_5$ and $B_6$ were $2.462mg{\cdot}100g^{-1}$ in fresh fatsia shoots (stem vegetables), and $0.127mg{\cdot}100g^{-1}$ in fresh spinach beet (leafy vegetables), respectively. Moreover, the vitamin $B_5$ and $B_6$ contents for parboiling treatment in most vegetables were reduced or not detected. In particular, the contents of vitamin $B_5$ in parboiled fatsia shoots and vitamin $B_6$ in parboiled yellow potato and spinach beet were decreased 20- and 4-fold compared with fresh material, respectively. These results can be used as important basic data for utilization and processing of various vegetable crops, information for dietary life, management of school meals, and national health for Koreans.

Analysis of Water Soluble Vitamin B1, B2, and B3 Contents in Korean Traditional Holiday Foods (우리나라 명절 및 제사음식에 함유된 수용성 비타민 B1, B2 및 B3의 함량 분석)

  • Kim, Gi-Ppeum;Hwang, Young-Sun;Choung, Myoung-Gun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.46 no.8
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    • pp.944-951
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    • 2017
  • This study aimed to determine and examine the contents of vitamins $B_1$, $B_2$, and $B_3$ using the high-performance liquid chromatography method in traditional holiday foods in Korea. All analyses were under the quality control chart of vitamins $B_1$, $B_2$, and $B_3$. The z-scores for vitamins $B_1$, $B_2$, and $B_3$ were 1.3, 0.0, and 0.6, respectively, in food analysis performance assessment scheme proficiency tests assuring reliability of analytical performance. Vitamin $B_1$, $B_2$, and $B_3$ contents were analyzed in a total of 31 samples. Vitamin $B_1$, $B_2$, and $B_3$ contents ranged from 0.000 to 0.973 mg/100 g, from 0.037 to 0.264 mg/100 g, and from 0.000 to 1.223 mg/100 g in Korean traditional holiday foods, respectively. The highest contents of vitamins $B_1$, $B_2$, and $B_3$ were 0.973 mg/100 g in Yukwon-jeon, 0.264 mg/100 g in Dongtae-jeon, and 1.223 mg/100 g in Yukwon-jeon sample, respectively. However, compared to vitamins $B_2$ and $B_3$, vitamin $B_1$ was not detected, generally. Therefore, these results can be used as basic data for a food composition table and improvement of national health for Koreans.

A Study of Current Status on Pesticide Residues in Commercial Dried Agricultural Products (서울시 유통 건조농산물 중의 농약잔류 실태 연구)

  • Kim, Bog-Soon;Park, Seoung-Gyu;Kim, Mi-Sun;Cho, Tae-Hee;Han, Chang-Ho;Jo, Han-Bin;Choi, Byung-Hyun;Kim, Sung-Dan
    • Korean Journal of Food Science and Technology
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    • v.39 no.2
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    • pp.114-121
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    • 2007
  • The purpose of this study was to investigate 253 kinds of pesticide residues in 58 commercial dried agricultural products in Seoul. The determinations of the pesticide residues were performed using multiresidue methods and were carried out by a gas chromatography-nitrogen phosphorus detector (GC-NPD), an electron capture detector ($GC-{\mu}ECD$), a mass spectrometry detector (GC-MSD) and high performance liquid chromatography-ultraviolet detector (HPLC-UV), and a fluorescence detector (HPLC-FLD). The pesticide residue detection rate in the commercial dried agricultural products was 24.1% (14 of 58 samples). Twelve pesticide residues without maximum residue limits (MRLs) were detected. In the vegetable groups, the frequency of pesticide residues was found to be in the increasing order of dried fruiting vegetables > dried leafy vegetables > dried stalk and stem vegetables. The pesticides used on dried red pepper in the dried fruiting vegetables were varied (7 kinds) and numerous (4 of 8 samples). The pesticide types detected in the commercial dried agricultural products were in the order of pyrethroid > organochloride > organophosphorus and insecticide > fungicide > herbicide ${\cdot}$ nematicide. The primary pyrethroid pesticide detected was cypermethrin. According to the producing areas of products, large numbers of pesticide residues were found in the order of Korea, China, North Korea, USA, and Vietnam.

Determination of the Levels of Bisphenol A Diglycidyl Ether (BADGE), Bisphenol F Diglycidyl Ether (BFDGE) and Their Reaction Products in Canned Foods Circulated at Korean Markets (캔 제품의 bisphenol A diglycidyl ether (BADGE), bisphenol F diglycidyl ether (BFDGE) 유도체 및 분해산물 분석법)

  • Kim, Hee-Yun;Lee, Jin-Sook;Cho, Min-Ja;Yang, Ji-Yeon;Baek, Ji-Yun;Cheong, So-Young;Choi, Sun-Hee;Kim, Young-Seon;Choi, Jae-Chun
    • Korean Journal of Food Science and Technology
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    • v.42 no.1
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    • pp.8-13
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    • 2010
  • Bisphenol A diglycidyl ether (BADGE) and bisphenol F diglycidyl ether (BFDGE) were obtained by a polymerization reaction of epichlorohydrin (ECH) with bisphenol A (BPA) or bisphenol F (BPF). These compounds are commonly used as monomers or additives such as a polymerization stabilizer and a hydrochloric acid scavenger of epoxy resin, polyvinyl chloride (PVC)-containing organosols and polyester lacquers, that are applied to the internal surface of most canned foods to impart chemical resistance. The unreacted BADGE, BFDGE and their reaction products migrating from epoxy resin, PVC-containing organosol and/or polyester lacquer-based food packaging materials into the foods have recently become an issue of great concern because of increased customer demand for safety. This study was conducted to develop a rapid and sensitive simultaneous analysis method based on HPLC/FLD and HPLC/APCI-mass and to evaluate the concentration of BADGE, BFDGE and their metabolites, BADGE $H_2O$, BADGE $2H_2O$, BADGE HCl, BADGE 2HCl, BADGE HCl $H_2O$, BFDGE $H_2O$, BFDGE $2H_2O$, BFDGE HCl, BFDGE 2HCl and BFDGE HCl $H_2O$ for 133 canned food samples. The method provided a linearity of 0.9997-0.9999, a limit of detection of $0.01-0.13\;{\mu}g/mL$, a limit of quantitation of $0.03-0.44\;{\mu}g/mL$ and a recovery (%) of 85.64-118.18. The number of samples containing BADGE, BFDGE or their metabolites were: 28/133 (21.1%), with levels of 0.400-0.888 mg/kg being observed for aqueous foods (19/133) and 0.093-0.506 mg/kg being observed for oily foods (9/133).

Examination of ivermectin residues in raw milk after skin administration (원유중 Ivermectin 구충제의 잔류실태 조사)

  • Bark, Jun-Jo;Youk, Ji-Hea;Kim, Hu-Kyoung;Park, Hye-Won;Kim, In-Kyung;Lee, Woo-Seong
    • Korean Journal of Veterinary Service
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    • v.30 no.3
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    • pp.421-428
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    • 2007
  • This study was conducted two kinds of aims: 1) to modify the analytical methods (conditions) by high performance liquid chromatography - fluorescence detector for the detection of residual ivermectin in raw milk, 2) to provide basic information for the evaluation of standard of the residual ivermectin in raw milk. It could be considerable that negative ion spectra can be better method in the LC/MS analysis for the detection of residues, Characteristic daughter ions were observed in negative ion spectra, however, linear line was not formed in positive ion one. Three Holstein cows ($500{\pm}10kg$) were applied to commercial ointment of ivermectin just one time at the first day of test, and residues in raw milk were examined for 20day after administration. The limit of detection (LOD) was 0.65ng (n=5) by HPLC/FLD, and recovery rates were $87.85%{\sim}99.47%$. The peak was observed at the 4th day, and residues lasted to the end. Thus ivermectin was prohibited when lactating.

Ingestion Exposure to Nitrosamines in Chlorinated Drinking Water

  • Kim, He-Kap;Han, Ki-Chan
    • Environmental Analysis Health and Toxicology
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    • v.26
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    • pp.2.1-2.7
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    • 2011
  • Objectives: N-Nitrosodimethylamine (NDMA) is classified as a probable human carcinogen by the United States Environmental Protection Agency (US EPA) and is formed during the chlorination of municipal drinking water. In this study, selected nitrosamines were measured in chlorinated drinking water collected from Chuncheon, Kangwon-do, Republic of Korea, and a risk assessment for NDMA was conducted. Methods: Twelve water samples were collected from 2 treatment plants and 10 household taps. Samples were analyzed for 6 nitrosamines via solid-phase extraction cleanup followed by conversion to dansyl derivatives and high-performance liquid chromatography-fluorescence detection (HPLC-FLD). Considering the dietary patterns of Korean people and the concentration change of NDMA by boiling, a carcinogenic risk assessment from ingestion exposure was conducted following the US EPA guidelines. Results: NDMA concentrations ranged between 26.1 and 112.0 ng/L. NDMA in water was found to be thermally stable, and thus its concentration at the end of boiling was greater than before thermal treatment owing to the decrease in water volume. The estimated excess lifetime carcinogenic risk exceeded the regulatory baseline risk of $10^{-5}$. Conclusions: This result suggests that more extensive studies need to be conducted on nitrosamine concentration distributions over the country and the source of relatively high nitrosamine concentrations.

Determination of Vitamin B6 Content using HPLC in Agricultural Products cultivated in Local Areas in Korea (HPLC를 이용한 지역 농산물의 비타민 B6 함량 분석)

  • Choi, So-Ra;Song, Eun-Ju;Song, Young-Eun;Choi, Min-Kyung;Han, Hyun-Ah;Lee, In-Sok;Shin, So-Hee;Lee, Ki-Kwon;Choi, Young-Min;Kim, Haeng-Ran
    • The Korean Journal of Food And Nutrition
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    • v.30 no.4
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    • pp.710-718
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    • 2017
  • Contents of water soluble vitamin $B_6$ in a total of 62 agricultural products cultivated in local areas in Korea were analyzed by high performance liquid chromatography with fluorescence detector (HPLC/FLD). To verify the method of vitamin $B_6$ analysis, a quality control chart was formulated with in-house control using a mixture of broccoli and shiitake mushrooms. Among cereals, high content of vitamin $B_6$ measured $234.3{\sim}260.3{\mu}g/100g$ in dried mung bean and soybean. Vitamin $B_6$ content of non-glutinous and glutinous black rice measured $105.0{\mu}g/100g$ and $129.7{\mu}g/100g$, respectively. In vegetables, high content of vitamin $B_6$ were measured in passion fruit ($104.3{\mu}g/100g$), gat ($55.7{\sim}84.3{\mu}g/100g$), gomchwi ($31.3{\sim}88.0{\mu}g/100g$) and garlic ($72.7{\sim}98.3{\mu}g/100g$). Among fruits, gold kiwi 'Zespri' and green kiwi 'Hayward' revealed high vitamin $B_6$ content of $116.3{\mu}g/100g$ and $78.7{\mu}g/100g$, respectively. In persimmons, daebongsi had high vitamin $B_6$ content ($36.0{\sim}72.7{\mu}g/100g$) than bansi and sweet persimmon. Vitamin $B_6$ content in dried jujube and persimmon increased more than $86.7{\mu}g/100g$ compared to fresh materials. Among specialty crops, green tea powder ($64.7{\sim}251.0{\mu}g/100g$) and sansuyu ($172.3{\mu}g/100g$) revealed high content. Of mushrooms, vitamin $B_6$ content of Sparassis crispa ($139.3{\mu}g/100g$) was the highest. Vitamin $B_6$ content information of agricultural products in local areas in Korea collected from this experiment will be used as valuable preliminary data for grasp national nutritional status.

Analysis of anatoxin-a in aqueous and cyanobacterial samples from korean lakes by liquid chromatography with fluorescence detection (액체크로마토그래피-형광검출법에 의한 호소시료의 아나톡신-a 분석)

  • Lee, In-Jung;Lee, Chul-Gu;Heo, Seong-Nam;Lee, Jae-Gwan
    • Analytical Science and Technology
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    • v.24 no.3
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    • pp.225-230
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    • 2011
  • Anatoxin-a is a cyanobacterial neurotoxin with a high toxicity produced by Anabaena, Aphanizomenon and Oscillatoria. Water bloom, formed by Anabaena has been occurring frequently in Lake Yeongchun. It is need to develop a sensitive method for determination of anatoxin-a to control potential hazard in raw water resources. In this study, we developed a highly sensitive analytical method of anatoxin-a using solid phase extraction (SPE) and high performance liquid chromatography (HPLC) with fluorescence detection. Anatoxin-a was converted into a highly fluorescent derivative using 4-fuoro-7-nitro-2,1,3-benzoxadiazole (NBF-F). The method was evaluated in terms of linearity of calibration curve, recovery and repeatability, and the adequate values were obtained. The method detection limit was $0.034\;{\mu}g/g$ and $0.022\;{\mu}g/L$ for algal and water samples, respectively. The concentrations of anatoxin-a were measured in algal and water samples from Lake Andong, Yeongchun and Daechung and ranged from $0.135\;{\mu}g/g$ to $10.979\;{\mu}g/g$ in algal samples and not detected in water samples.