• Title/Summary/Keyword: LC-PDA/MS/MS

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Screening of anti-obesity drugs, their analogues and prohibited ingredients in slimming foods (식품 중 부정 혼입된 비만치료제 및 사용금지 성분 실태조사)

  • Yun, Jisuk;Choi, Jangduck;Kwon, Kisung;Jo, Cheon-Ho
    • Korean Journal of Food Science and Technology
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    • v.48 no.5
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    • pp.424-429
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    • 2016
  • Globally, obesity has been recognized as a serious health problem. Recently, slimming foods for weight loss and maintenance were found to contain anti-obesity drugs, their analogues, and prohibited ingredients. To avoid inspections by the Government, structurally modified analogs have been continuously synthesized. For rapid determination of adulterated slimming products, we simultaneously analyzed 21 illegal compounds using liquid chromatography (LC) equipped with photo diode array, and LC coupled with tandem mass spectrometry. The validation of the method was performed with regard to selectivity, linearity, limit of detection, limit of quantification, precision, and accuracy. We purchased 128 samples from the Korean market and online sources in the year 2015. In 31 samples, 3 illegal compounds were detected as follows: 9.9-135.3 mg/g of sibutramine, 0.2-17.5 mg/g of yohimbine, and 1.8 mg/g of icariin. This simultaneous detection method might prove to be a simple and rapid analysis for monitoring illegal compounds in slimming foods.

The Optimization and Verification of an Analytical Method for Sodium Iron Chlorophyllin in Foods Using HPLC and LC/MS (식품 중 철클로로필린나트륨의 HPLC 및 LC/MS 최적 분석법과 타당성 검증)

  • Chong, Hee Sun;Park, Yeong Ju;Kim, Eun Gyeom;Park, Yea Lim;Kim, Jin Mi;Yamaguchi, Tokutaro;Lee, Chan;Suh, Hee-Jae
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.148-157
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    • 2019
  • An optimized analytical method for sodium iron chloriphyllin in foods was established and verified by using high performance liquid chromatography with attached diode array detection. An Inertsil ODS-2 column and methanol-water (80:20 containing 1% acetate) as a mobile phase were employed. The limit of detection and quantitation of sodium iron chloriphyllin were 0.1 and 0.3 mg/kg, respectively, and the linearity of calibration curve was excellent ($R^2=0.9999$). The accuracy and precision were 93.9~104.95% and 2.0~7.7% in both inter-day and intra-day tests. Recoveries for candy and salad dressing were ranged between 93 and 104% (relative standard deviation, (RSD) 0.3~4.3%), and between 83 and 115% (RSD 1.2~2.0%), respectively. Liquid chromatography mass spectrometry was used to verify the main components of sodium iron chlorophyllin which were Fe-isochlorin e4 and Fe-chlorin e4.

A Survey on the Pesticide Residues and Risk Assessment for Agricultural Products on the Markets in Incheon Area from 2010 to 2012 (인천광역시 유통 농산물의 최근 3년간의 잔류농약 실태 및 안전성 조사)

  • Kim, Hye-Young;Lee, Soo-Yeon;Kim, Cheol-Gi;Choi, Eun-Jeong;Lee, Eun-Ju;Jo, Nam-Gyu;Lee, Jea-Man;Kim, Yong-Hee
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.61-69
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    • 2013
  • BACKGROUND: This survey was done to investigate the pesticide residues and to assess their risk on agricultural products on the Markets in Incheon from 2010 to 2012. METHODS AND RESULTS: The total number of samples were 16,025 for agricultural products and these were analyzed by multi-residue method using GC-ECD/NPD, GC-MS, LC-MS/MS and HPLC-PDA/FLD. The violation rates of the samples over maximum residue limits(MRLs) of pesticide residues established by Korean Food and Drug Administration in the survey of 2010, 2011 and 2012 were 1.2%, 0.8% and 0.7%, respectively. CONCLUSION(S): Of the total violated samples, more than 75% of the rates were recorded from the samples of leafy vegetables. Most commonly encountered agricultural commodities over MRLs were Chwinamul, perilla leaves and crown daisy. The pesticides detected yearly over MRLs during three years were endosulfan, chlorpyrifos, diazinon, lufenuron, chlorothalonil, flutolanil, procymidone, ethoprophos. Estimated daily intakes compared to acceptable daily intakes, except radish and Welsh onion, is estimated less harm on human in 10 kinds of pesticides which frequently occurred violation.

Monitoring and Safety Assessment of Pesticide Residues and Sulfur Dioxide on Functional Rice Products (기능성 쌀의 잔류농약 및 이산화황 안전성 실태조사)

  • Lee, You-Jin;Park, Myung-Ki;Kim, Ki-Yu;Park, Eun-Mi;Kang, Heung-Gyu;Lim, Ji-Hyun;Cho, Wook-Hyun;Kim, Youn-Ho;Lee, Sun-Young;Yong, Kum-Chan;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.32 no.6
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    • pp.493-499
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    • 2017
  • This study was conducted to monitor the current status of pesticide residues and sulfur dioxide in a total of 91 functional rice products from February to October 2016. Multi class pesticide multiresidue methods of 220 pesticides was performed by the GC/ECD, GC/NPD, GC/TOF/MS, LC/PDA, and LC/FLD. As a result of analysis, the pesticides were detected in 3 samples, representing a detection rate of 3.3%. The kind of pesticides was propiconazole and isoprothiolane used for germicide in agriculture or plant growth regulator purposes. The detected levels were 0.0340~0.0566 mg/kg, which were under the MRL (Maximum Residues Limits). The contents of sulfur dioxide in 91 samples by the Monier-Williams method were not detected. Risk assessment of pesticides evaluated using human health exposure with the ratio of EDI (Estimated daily intake) to ADI (Acceptable daily intake). %ADI (the ratios of EDI to ADI) were 0.24~1.25% with safety level.

Development and validation of an analytical method for the determination of lepimectin residues by HPLC-PDA (HPLC-PDA를 이용한 lepimectin 잔류량 분석법 개발 및 확인)

  • Do, Jung-Ah;Kwon, Ji-Eun;Kim, Mi-Ra;Lee, Eun-Mi;Kuk, Ju-Hee;Kwon, Kisung;Oh, Jae-Ho
    • Analytical Science and Technology
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    • v.26 no.2
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    • pp.142-153
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    • 2013
  • A new, rapid, and simple analytical method was developed and validated using high performance liquid chromatograph-photodiode array detector (HPLC-PAD) for the determination of lepimectin residues in agricultural commodities. The lepimectin residues in samples were extracted with methanol, partitioned with dichloromethane, and then purified with glass column filled with subsequently to aminopropyl ($NH_2$) solid phase extraction (SPE) cartridge. The purified samples were detected using HPLC-PAD. Correlation coefficient ($R^2$) of both lepimectin $A_3$ and $A_4$ solutions were 0.9999. The method was validated using cucumber spiked with lepimectin at 0.02 and 0.2 mg/kg and pepper, mandarin, hulled rice, potato, soybean at 0.02 and 0.5 mg/kg. Average recoveries were 76.0~114.8% with relative standard deviation less than 10%, and limit of detection (LOD) and limit of quantification (LOQ) were 0.005 and 0.01 mg/kg, respectively. The result of recoveries and overall coefficient of variation of a laboratory results in Gwangju regional KFDA and Daejeon regional KFDA was followed with Codex guideline (CAC/GL 40). Therefore, developed method in this study is accurate, rapid, and appropriate for lepimectin determination and will be used to keep safety of lepimectin residues in agricultural products.

Quantitative Analysis about Phenolic Compounds of Dendranthema Species in Korean Native Plants (국내 자생 구절초속 중 페놀화합물 함량분석)

  • Kim, Kyeong Mi;Lee, Seon Yu;Jo, Ara;Kang, Byoung Man;Ham, Seongho;Cho, Junghee;Lee, Gukyeo
    • Korean Journal of Pharmacognosy
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    • v.48 no.1
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    • pp.70-76
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    • 2017
  • Dendranthema spp are distributed in various regions in Korea. This report is the quantitative results of phenolic compounds on the 5 resources collected from all over the country. It was known that it has phenolic compounds, as an anticoagulant activities and immunoadjuvant activity of contribute to the cardiovascular effects. This was used for quantitative analysis of chlorogenic acid(CA), 3,5-Dicaffeoylquinic acid(3,5-DCA), 4,5-Dicaffeoylquinic acid(4,5-DCA) and linarin, with UPLC-PDA and LC-IT-TOF-MS. Extraction efficiency of compounds was compared by using ultrasonic extraction and reflux extraction with different extraction conditions (methods and time). In 50% MeOH extracs (30 mins) of Dendranthema zawadskii (Herb.) Tzvelev (SDZ), Dendranthema zawadskii var. yezoense (Maek.) Y.M.Lee & H.J.Choi (NDZ), Dendranthema zawadskii (Herb.) Tzvelev var. teuisectum (Kitag.) J. H. Pak (GDZ), Dendranthema careanum (H. $L{\acute{e}}v$. & Vaniot) Vorosch. (HDC) and Dendranthema zawadskii var. tenuisectum Kitag (PDZ), chlorogenic acid contents were 1.14‰, 6.95‰, 7.27‰, 1.47‰ and 2.64‰, 3,5-dicaffeoylquinic acid contents were 3.30‰, 5.60‰, 10.81‰, 2.67‰ and 1.50‰, 4,5-dicaffeoylquinic acid contents were 0.74‰, 1.93‰, 3.36‰, 0.61‰ and 0.43‰ and linarin contents were 3.90‰, 10.15‰, 0.15‰, 0.73‰ and 0.21‰, respectively.

Development and Validation of an Analytical Method for Ametoctradin Residue Determination in Domestic Agricultural Commodities by HPLC-PDA (HPLC-PDA를 이용한 국내 유통 농산물 중 ametoctradin 잔류량 분석법 개발 및 검증)

  • Do, Jung-Ah;Kwon, Ji-Eun;Lee, Eun-Mi;Kim, Mi-Ra;Kuk, Ju-Hee;Cho, Yoon-Jae;Kang, Il-Hyun;Kim, Hyung-Su;Kwon, Kisung;Oh, Jae-Ho
    • Korean Journal of Food Science and Technology
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    • v.45 no.3
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    • pp.285-292
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    • 2013
  • This study was carried out to validate the safety of ametoctradin residues in agricultural commodities by developing an official analysis method. An analytical method was developed and validated using HPLC-PDA detectors. The samples were extracted with methanol, subsequently partitioned with dichloromethane and purified with florisil column chromatograph using acetone/hexane (30/70, v/v) as solvent. The method was validated by using grape, hulled rice, mandarin, and potato spiked with ametoctradin at 0.05 and 5.0 mg/kg, and pepper at 0.05 and 2.0 mg/kg. Average recoveries were 76-114.8% with relative standard deviation less than 10%, and the limit of detection and limit of quantification were 0.0125 and 0.05 mg/kg, respectively. The result of recoveries and overall coefficient of variation of the laboratory results from Gwangju regional Food and Drug Administration (FDA) and Daejeon regional FDA was accorded with Codex Alimentarius Commission Guideline (CAC/GL 40). Based on these results, this method was found to be appropriate for ametoctradin residue determination and can be used as the official method of analysis.

Multi-residue Pesticide Analysis in Cereal using Modified QuEChERS Samloe Preparation Method (곡물류 중 잔류농약 다성분 분석을 위한 개선된 QuEChERS 시료 정제법의 개발)

  • Yang, In-Cheol;Hong, Su-Myeong;Kwon, Hye-Young;Kim, Taek-Kyum;Kim, Doo-Ho
    • The Korean Journal of Pesticide Science
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    • v.17 no.4
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    • pp.314-334
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    • 2013
  • This study explored an efficient modified Quick, Easy, Cheap, Effective, Rugged and safe (QuEChERS) method combined with liquid chromatography-electrospray ionization with tandem mass spectrometric detection for the analysis of residues of 76 pesticides in brown rice, barley and corn including acidic sulfonylurea herbicides. Formic acid (1%) acid in acetonitrile and dispersive solid phase extractions used for extraction of pesticides and clean-up of the extract respectively. Two fortified spikes at 50 and 200 ng $g^{-1}$ levels were performed for recovery test. Mean recoveries of majority of pesticides at two spike levels ranged from 73.2 to 132.2, 80.9 to 136.8, 66.6 to 143.5 for brown rice, barley and corn respectively with standard error (CV) less than 10%. Good linearity of calibration curves were achieved with $R^2$ > 0.9907 within the observed concentration ranged. The modified method also provided satisfactory results for sulfonylurea herbicides. The method was applied to the determination of residues of target pesticides in real samples. A total of 26 pesticides in 36 out of 98 tasted samples were observed. The highest concentration was observed for tricyclazole at 1.17 mg $kg^{-1}$ in brown rice. This pesticide in two brown rice samples exceeded their MRLs regulated for rice in republic of Korea. Except tricyclazole none of the observed pesticides' concentration was higher than their MRLs. The results reveal that the method is effectively applicable to routine analysis of residues of target pesticides in brown rice, barley and corn.

Comparison of the bioactive compounds and anti-inflammatory effects found in different flower colors from Abeliophyllum distichum Nakai (미선나무 꽃 색에 따른 생리활성 화합물 및 항염증 활성 비교)

  • Jang, Tae-Won;Choi, Ji-Soo;Han, So-Yeon;Park, Hye-Jeong;Lee, Da-Yoon;Min, Young-Sil;Park, Jae-Ho
    • Journal of Applied Biological Chemistry
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    • v.65 no.3
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    • pp.203-213
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    • 2022
  • Abeliophyllum distichum (A. distichum, Korean endemic plant) is one genus and one species in the Oleaceae family. According to the color variation of petals and calyx, A. distichum is classified as A. distichum (white flower), A. distichum for. lilacinum (pink flowers), A. distichum for. eburneum (ivory flowers), and Okhwang 1 (golden flowers). In previous studies, bioactivities (antioxidant, anti-inflammatory, and anti-cancer) of A. distichum have been reported. We conducted a comparison of the differences in bioactive compounds and the anti-inflammatory effects on macrophages among four flowers of A. distichum (FAD). The identification and quantification of glycosides were analyzed by HPLC/PDA and LCMS. These results were shown FAD has rutin, hirsutrin, and acteoside. Antioxidant activity of FAD significantly decreased reactive oxygen species. In addition, FAD reduced the expression of pro-inflammatory mediators (nitric oxide, iNOS, and COX-2) in lipopolysaccharide-induced RAW 264.7 cells. For further study, we investigated the regulation of nuclear factor kappa B (NF-κB) and mitogen-activated protein kinase (MAPK) signaling pathways. In conclusion, FAD may exert anti-inflammatory effects by suppressing inflammatory mediators via regulations of NF-κB and MAPK signaling pathways. Therefore, these findings suggest that FAD is a potential resource as a preventative or therapeutic agent for inflammation.