• Title/Summary/Keyword: Adulteration

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Simultaneous Determination of 80 Unapproved Compounds using HPLC and LC-MS/MS in Dietary Supplements

  • Kwon, Jeongeun;Shin, Dasom;Kang, Hui-Seung;Suh, Junghyuck;Lee, Gunyoung;Lee, Eunju
    • Mass Spectrometry Letters
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    • v.13 no.3
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    • pp.58-83
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    • 2022
  • We developed analytical methods using high performance chromatography (HPLC) and liquid chromatography tandem mass spectrometry (LC-MS/MS) for the simultaneous determination of 80 unapproved compounds in dietary supplements. The target compounds for analysis were unapproved ingredients (e.g., pharmaceuticals) that have potential adverse effects on consumers owing to accidental misuse, overuse, and interaction with other medication in dietary supplement. Two analytical methods were tested to identify the optimal validation results according to AOAC guideline. As a result, limit of quantification (LOQ) was 0.14-0.5 ㎍ mL-1; linearity (r2) was ≥ 0.99; accuracy (expressed as recovery) was 78.9-114%; precision (relative standard deviation) was ≤ 4.28% in the HPLC method. In the LC-MS/MS method, LOQ was 0.01-2 ng mL-1, linearity (r2) was ≥0.98, accuracy was 71.7-119%; precision was ≤ 12.5%. The developed methods were applied to 51 dietary supplements collected from 2019 to 2021 through MFDS alert system. Based on our previous monitoring study, major compounds were icariin, sibutramine, yohimbine, sildenafil, tadalafil, sennosides (A, B), cascarosides (A, B, C, D), and phenolphthalein. In this study, we re-analyzed samples of detected compounds, and evaluated the statistical difference using Bland-Altman analysis to compare two analytical approaches between HPLC and LC-MS/MS. These results showed a good agreement between two methods that can be used to monitor the unapproved ingredients in dietary supplements. The developed two methods are complementarily suitable for monitoring the adulteration of 80 unapproved compounds in dietary supplements.

Discrimination of vegetable oils by stable carbon isotope ratio and fatty acid composition (탄소 안정동위원소 비율 및 지방산 조성을 활용한 식용유지류의 판별)

  • Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik;Cho, Yoon-Jae;Chae, Young-Sik
    • Analytical Science and Technology
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    • v.27 no.1
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    • pp.66-77
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    • 2014
  • This study was carried out to examine the authenticity discrimination of circulated vegetable oils by using carbon isotope ratio (${\delta}^{13}C$) and fatty acid composition. This analysis was applied to vegetable oils which we can buy in Korean markets, and the analytical instrument was measured by using EA-IR/MS for ${\delta}^{13}C$ and GC/FID for fatty acid composition. ${\delta}^{13}C$ was separated into 3 groups as $C_3$ plant including sesame oil, $C_4$ plant including maize oil, and rice bran oil. Fatty acid composition was significantly different among vegetable oils. In addition, the interval of low and high price vegetable oils was classified through the scatter plot analysis showing the correlation of the ${\delta}^{13}C$ and fatty acid composition. Therefore, through a simultaneous determination of the ${\delta}^{13}C$ and fatty acid composition, we are able to determine the majority of vegetable oils. It help to ensure food safety in Korean market by exclusion of economically modified adulteration in food.

Development of the Duplex PCR Method of Identifying Trachurus japonicus and Trachurus novaezelandiae (다중 PCR 분석법을 이용한 전갱이속 어종의 신속한 종판별 분석법 개발)

  • Park, Yeon Jung;Lee, Mi Nan;Kim, Eun Mi;Noh, Eun Soo;Noh, Jae Koo;Park, Jung Youn;Kang, Jung-Ha
    • Journal of Life Science
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    • v.28 no.9
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    • pp.1062-1067
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    • 2018
  • Reliable labeling of fish products can reassure consumers regarding the identity and quality of seafoods. Therefore, techniques that can identify adulteration or mislabeling are valuable. To rapidly identify two Trachurus species, Trachurus japonicus and Trachurus novaezelandiae, a highly efficient, rapid, duplex polymerase chain reaction (PCR) having two species-specific primers simultaneously was identified. This species-specific primer focused on a single nucleotide mismatch in the 3'-terminal base of a primer designed in the mitochondrial cytochrome c oxidase (COI) subunit I DNA. To optimize the duplex PCR condition, gradient PCR reactions were conducted to determine the primer annealing temperature and the primer concentration. The PCR's product was observed on the gel, suggesting that DNA molecules may be useful in differentiating the two species. The length of the amplification fragments were 103 bp for Trachurus japonicus and 214 bp for Trachurus novaezelandiae, which, along with the species-specific primer visualized by agarose gel electrophoresis, enabled accurate distinction of the species of the Trachurus genus. These results indicate that the duplex PCR, which has a species-specific primer based on single nucleotide polymorphism (SNP), can be useful for rapidly differentiating the two species of Trachurus. This duplex PCR analysis is simple, rapid, and reliable, and could be beneficial to protecting consumers' rights.

Development of Nondestructive Detection Method for Adulterated Powder Products Using Raman Spectroscopy and Partial Least Squares Regression (라만 분광법과 부분최소자승법을 이용한 불량 분말식품 비파괴검사 기술 개발)

  • Lee, Sangdae;Lohumi, Santosh;Cho, Byoung-Kwan;Kim, Moon S.;Lee, Soo-Hee
    • Journal of the Korean Society for Nondestructive Testing
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    • v.34 no.4
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    • pp.283-289
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    • 2014
  • This study was conducted to develop a non-destructive detection method for adulterated powder products using Raman spectroscopy and partial least squares regression(PLSR). Garlic and ginger powder, which are used as natural seasoning and in health supplement foods, were selected for this experiment. Samples were adulterated with corn starch in concentrations of 5-35%. PLSR models for adulterated garlic and ginger powders were developed and their performances evaluated using cross validation. The $R^2_c$ and SEC of an optimal PLSR model were 0.99 and 2.16 for the garlic powder samples, and 0.99 and 0.84 for the ginger samples, respectively. The variable importance in projection (VIP) score is a useful and simple tool for the evaluation of the importance of each variable in a PLSR model. After the VIP scores were taken pre-selection, the Raman spectrum data was reduced by one third. New PLSR models, based on a reduced number of wavelengths selected by the VIP scores technique, gave good predictions for the adulterated garlic and ginger powder samples.

Thermal Stable Soluble Proteins in Pork Fat and Meat, and Their Antigenicity (돈지육 및 돈육 중 열안정성 단백질의 존재 확인과 이의 항원성 확인)

  • Kim, Jeong-Sook;Lee, Jeong-Eun;Shim, Won-Bo
    • Journal of Food Hygiene and Safety
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    • v.31 no.6
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    • pp.445-450
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    • 2016
  • Thermal-stable soluble proteins (TSSP) in livestock products has been recently reported. Therefore, the development of antibodies and immunoassay using a TSSP is useful because the presence of TSSP can be measured on processed food. In this study, the existence of TSSPs in pork fat and meat was confirmed and their antigenicity was investigated. The extracts from pork fat and meat by heating method were analyzed by SDS-PAGE with 5% stacking and 12% separating gels. The protein profiles from the raw pork fat and meat extracts (major band ranged 25 to 100 kDa) without cooking and heating treatments were significantly different compared to those from cooked and heated pork fat and meat extracts (several major bands > 100 kDa and < 30 kDa). This meant that non thermal-stable soluble proteins ranged from 25 to 100 kDa may be denaturated to insoluble proteins by cooking and heating treatments, and TSSPs were in pork fat and meat at kept their properties. The confirmed TSSPs were used as an immunogen to investigate their antigenicity. Eight mice (5 mice for pork fat and 3 mice for pork meat) were separately immunized with the TSSPs of pork fat and meat, and the anti-sera obtained from the immunized mice showed high titer values. Polyclonal antibodies against each target protein showed the specific reaction to pork fat and meat, individually. These indicated that TSSP could be used as an immunogen to produce antibodies such as monoclonal and polyclonal antibodies. In addition, antibodies specific to TSSP from pork fat and meat may be used as a bio-receptor in immunoassays for the identification of fraudulent adulteration with pork fat and meat in livestock products.

Rapid Gas Chromatographic Screening of Vegetable Oils for Free Fatty Acids (기체크로마토그래피법에 의한 식물성 유지내 유리 지방산의 신속한 스크리닝)

  • Kim, Jung-Han;Kim, Kyoung-Rae;Chai, Jeong-Young;Oh, Chang-Hwan;Park, Hyung-Kook
    • Korean Journal of Food Science and Technology
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    • v.25 no.4
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    • pp.373-378
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    • 1993
  • A rapid gas chromatographic profiling method for the simultaneous analysis of free fatty and other acids was applied to vegetable oils. Oil samples were dissolved in dichloromethane and the free acids were extracted with saturated $NaHCO_3$ solution. The aqueous extract was acidified and then loaded onto the Chromosorb P column for the extraction. The acids were eluted with diethyl ether selectively from Chromosorb P column and were treated with triethylamine to prevent the losses of volatile acids. Several long chain fatty acids were detected from soybean oil, rice-bran oil, sesame oil and perilla oil. Various organic acids including odd number fatty acids were detected in crude oil, especially sesame oil. Arachidic acid from perilla oil and vanillic acid from sesame oil, which were not reported before were detected. The content ratio of free linoleic acid to oleic acid was $1.02{\sim}1.18$, which was similar to the reported data. When the GC profile of organic acids were simplified to their corresponding retention index spectra of bar graphical forms, they presented characteristic pattern of each vegetable oil that can be quickly recognized.

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Detection of the Adulterated Sesame Oil by the Analysis of Fatty Acid Compositions and Carbon Isotope Ratio (지방산조성과 탄소동위원소 분석에 의한 참기름에 혼입된 타식용유의 검출방법)

  • Ha, Jae-Ho;Hawer, Woo-Derck;Hwang, Jin-Bong
    • Korean Journal of Food Science and Technology
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    • v.25 no.4
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    • pp.345-350
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    • 1993
  • Fatty acid composition of sesame oil could be distinguished from that of rapeseed oil and soybean oil by the content of linolenic acid. The relative composition of each fatty acid revealed the clear difference between sesame oil and other vegetable oils except corn oil. Ricebran oil was different from sesame oil in the relative composition of palmitic acid with respect to stearic acid and cottonseed oil in oleic acid to linoleic acid. ${\delta}^{13}C$ of corn oil was $19.40%_{\circ}$, in oleic acid and $-17.11%_{\circ}$, in linoleic acid, while that of sesame oil was $-27.60%_{\circ}$ in oleic acid and $-27.70%_{\circ}$ in linoleic acid. Therefore, most adulterant could be detected by comparing the ratio of fatty acids in vegetable oils except corn oil. It could, however, be detected by comparing carbon isotope ratio in the case of corn oil.

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Characteristics of Silica Coated ${\gamma}-Fe_{2}O_{3}$ with Heat-treatment (열처리에 따른 실리카 피착 ${\gamma}-Fe_{2}O_{3}$의 특성)

  • Lee, J.Y.;Byeon, T.B.;Kim, D.Y.;Lee, H.;Han, K.H.;Sohn, J.G.
    • Journal of the Korean Magnetics Society
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    • v.3 no.2
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    • pp.108-114
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    • 1993
  • This paper presents a study on the effects of silica coating in the production of ${\gamma}-Fe_{2}O_{3}$ powders suitable for magnetic recording media. Emphasis has been put on investigating the relationship between the powder characteristics and the effects of silica coating in the heat-treatment stage of ${\gamma}-Fe_{2}O_{3}$ production. After we prepared non-coated ${\gamma}-Fe_{2}O_{3}$ and silica coated ${\gamma}-Fe_{2}O_{3}$ with coating water glass on the surface of goethite and heattreatment process, we compared and investigated powder characteristics. As silica coated layer played a role of preventing the powders from overreduction to metal iron and rapid oxidation, silica coated ${\gamma}-Fe_{2}O_{3}$ showed superior magnetization value due to inhibiting t!1e adulteration of ${\alpha}-Fe_{2}O_{3}$ into the final product. When silica coated layer acted as a sintering restrainer, silica coated ${\gamma}-Fe_{2}O_{3}$ showed high coercivity and specific sur-face area due to good acicularity.

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Simultaneous determination of Phlomis umbrosa and Dipsacus asperoides in foods using LC-MS/MS methods (LC-MS/MS를 이용한 식품 중 천속단과 한속단 지표성분 동시분석)

  • Yun, Jisuk;Kim, Jinyoung;Choi, Jangduck;Kwon, Kisung;Jo, Cheon-Ho
    • Korean Journal of Food Science and Technology
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    • v.48 no.6
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    • pp.531-535
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    • 2016
  • Phlomis umbrosa and Dipsacus asperoides are distinct species, even though they have a similar appearance. Dipsacus asperoides is used as a Chinese medicinal plant for and has bone strengthening and fracture healing but Phlomis umbrosa has no effect on bone growth. Recently, these plants were used in children's food to improve their bone growth, without distinction in food. Intakes of Dipsacus asperoides in food may be dangerous, because it has never been used in food and its safety has never been tested in humans. We developed liquid chromatography with tandem mass spectrometry method to distinguish these plants in food. The method was validated for linearity, limits of detection, limits of quantification, accuracy and precision. In 5 of 17 samples, we identified Dipsacus asperoides, containing loganin $0.19-14.45{\mu}g/mL$, sweroside $0.13-4.61{\mu}g/mL$ and akebia saponin D $0.59-19.29{\mu}g/mL$. The developed method might be useful to identify Dipsacus asperoides in adulterated food.

MAKING AGRICULTURAL INSURANCE IN INDIA FARMER-FRIENDLY AND CLIMATE RESILIENT

  • Kumar, K. Nirmal Ravi
    • Agribusiness and Information Management
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    • v.11 no.1
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    • pp.27-39
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    • 2019
  • Agricultural risks are exacerbated by a variety of factors ranging from climatevariability and change, frequent natural disasters, uncertainties in yields and prices, weakrural infrastructure, imperfect markets and lack of financial services including limited spanand design of risk mitigation instruments such as credit and insurance. Indian agriculture has little more than half (53%) of its area still rainfed and this makes it highly sensitive to vagaries of climate causing unstable output. Besides adverse climatic factors, there are man-made disasters such as fire, sale of spurious seeds, adulteration of pesticides and fertilizers etc., and all these severely affect farmers through loss in production and farm income, and are beyond the control of farmers. Hence, crop insurance' is considered to be the promising tool to insulate the farmers from risks faced by them and to sustain them in the agri-business. This paper critically evaluates the performance of recent crop insurance scheme viz., Pradhan Mantri Fasal Bhima Yojana (PMFBY) and its comparative performance with earlier agricultural insurance schemes implemented in the country. It is heartening that, the comparative performance of PMFBY with earlier schemes revealed that, the Government has definitely taken a leap forward in covering more number of farmers and bringing more area under crop insurance with the execution of this new scheme and on this front, it deserves the appreciation in fulfilling the objective for bringing more number of farmers under insurance cover. The use of mobile based technology, reduced number of Crop Cutting Experiments (CCEs) and smart CCEs, digitization of land record and linking them to farmers' account for faster assessment/settlement of claims are some of the steps that contributed for effective implementation of this new crop insurance scheme. However, inadequate claim payments, errors in loss/yield assessment, delayed claim payment, no direct linkage between insurance companies and farmers are the major shortcomings of this scheme. This calls for revamping the crop insurance program in India from time to time in tune with the dynamic changes in climatic factors on one hand and to provide a safety-net for farmers to mitigate losses arising from climatic shocks on the other. The future research avenues include: insuring the revenue of the farmer (Price × Yield) as in USA and more and more tenant farmers should be brought under insurance by doling out discounts for group coverage of farmers like in Philippines where 20 per cent discount in premium is given for a group of 5-10 farmers, 30 per cent for a group of 10-20 and 40 per cent for a group of >20 farmers.