• Title/Summary/Keyword: Magnesium Sulfate

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Development and Validation of a Simultaneous Analytical Method for 5 Residual Pesticides in Agricultural Products using GC-MS/MS (GC-MS/MS를 이용한 농산물 중 잔류농약 5종 동시시험법 개발 및 검증)

  • Park, Eun-Ji;Kim, Nam Young;Shim, Jae-Han;Lee, Jung Mi;Jung, Yong Hyun;Oh, Jae-Ho
    • Journal of Food Hygiene and Safety
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    • v.36 no.3
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    • pp.228-238
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    • 2021
  • The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. The extracts were cleaned up using MgSO4, primary secondary amine (PSA) and octadecyl (C18). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R2) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).

Improvement of an Analytical Method for Methoprene in Livestock Products using LC-MS/MS (LC-MS/MS를 이용한 축산물 중 살충제 메토프렌의 잔류분석법 개선)

  • Park, Eun-Ji;Kim, Nam Young;Park, So-Ra;Lee, Jung Mi;Jung, Yong Hyun;Yoon, Hae Jung
    • Journal of Food Hygiene and Safety
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    • v.37 no.3
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    • pp.136-142
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    • 2022
  • The research aims to develop a rapid and easy analytical method for methoprene using liquid chromatography-tandem mass spectrometry (LC-MS/MS). A simple, highly sensitive, and specific analytical method for the determination of methoprene in livestock products (beef, pork, chicken, milk, eggs, and fat) was developed. Methoprene was effectively extracted with 1% acetic acid in acetonitrile and acetone (1:1), followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium acetate. Subsequently, the lipids in the livestock sample were extracted by freezing them at -20℃. The extracts were cleaned using MgSO4, primary secondary amine (PSA), and octadecyl (C18), which were then centrifuged to separate the supernatant. Nitrogen gas was used to evaporate the supernatant, which was then dissolved in methanol. The matrix-matched calibration curves were constructed using 8 levels (1, 2.5, 5, 10, 25, 50, 100, 150 ng/mL) and the coefficient of determination (R2) was above 0.9964. Average recoveries spiked at three levels (0.01, 0.1, and 0.5 mg/kg), and ranged from 79.5-105.1%, with relative standard deviations (RSDs) smaller than 14.2%, as required by the Codex guideline (CODEX CAC/GL 40). This study could be useful for residue safety management in livestock products.

Development of a Simultaneous Analytical Method for Azocyclotin, Cyhexatin, and Fenbutatin Oxide Detection in Livestock Products using the LC-MS/MS (LC-MS/MS를 이용한 축산물 중 유기주석계 농약 Azocyclotin, Cyhexatin 및 Fenbutatin oxide의 동시시험법 개발)

  • Nam Young Kim;Eun-Ji Park;So-Ra Park;Jung Mi Lee;Yong Hyun Jung;Hae Jung Yoon
    • Journal of Food Hygiene and Safety
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    • v.38 no.5
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    • pp.361-372
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    • 2023
  • Organotin pesticide is used as an acaricide in agriculture and may contaminate livestock products. This study aims to develop a rapid and straightforward analytical method for detecting organotin pesticides, specifically azocyclotin, cyhexatin, and fenbutatin oxide, in various livestock products, including beef, pork, chicken, egg, and milk, using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The extraction process involved the use of 1% acetic acid in a mixture of acetonitrile and ethyl acetate (1:1). This was followed by the addition of anhydrous magnesium sulfate (MgSO4) and anhydrous sodium chloride. The extracts were subsequently purified using octadecyl (C18) and primary secondary amine (PSA), after which the supernatant was evaporated. Organotin pesticide recovery ranged from 75.7 to 115.3%, with a coefficient of variation (CV) below 25.3%. The results meet the criteria range of the Codex guidelines (CODEX CAC/GL 40). The analytical method in this study will be invaluable for the analysis of organotin pesticides in livestock products.

Development and Validation of the Analytical Method for Oxytetracycline in Agricultural Products using QuEChERS and LC-MS/MS (QuEChERS법 및 LC-MS/MS를 이용한 농산물 중 Oxytetracycline의 잔류시험법 개발 및 검증)

  • Cho, Sung Min;Do, Jung-Ah;Lee, Han Sol;Park, Ji-Su;Shin, Hye-Sun;Jang, Dong Eun;Cho, Myong-Shik;Jung, ong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.3
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    • pp.227-234
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    • 2019
  • An analytical method was developed for the determination of oxytetracycline in agricultural products using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method by liquid chromatography-tandem mass spectrometry (LC-MS/MS). After the samples were extracted with methanol, the extracts were adjusted to pH 4 by formic acid and sodium chloride was added to remove water. Dispersive solid phase extraction (d-SPE) cleanup was carried out using $MgSO_4$ (anhydrous magnesium sulfate), PSA (primary secondary amine), $C_{18}$ (octadecyl) and GCB (graphitized carbon black). The analytes were quantified and confirmed with LC-MS/MS using ESI (electrospray ionization) in positive ion MRM (multiple reaction monitoring) mode. The matrix-matched calibration curves were constructed using six levels ($0.001{\sim}0.25{\mu}g/mL$) and coefficient of determination ($r^2$) was above 0.99. Recovery results at three concentrations (LOQ, $10{\times}LOQ$, and $50{\times}LOQ$, n=5) were from 80.0 to 108.2% with relative standard deviations (RSDs) less than of 11.4%. For inter-laboratory validation, the average recovery was in the range of 83.5~103.2% and the coefficient of variation (CV) was below 14.1%. All results satisfied the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for oxytetracycline determination in agricultural commodities. This study could be useful for safety management of oxytetracycline residues in agricultural products.

Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살충제 Broflanilide 및 대사물질 동시시험법 개발)

  • Park, Ji-Su;Do, Jung-Ah;Lee, Han Sol;Park, Shin-min;Cho, Sung Min;Kim, Ji-Young;Shin, Hye-Sun;Jang, Dong Eun;Jung, Yong-hyun;Lee, Kangbong
    • Journal of Food Hygiene and Safety
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    • v.34 no.2
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    • pp.124-134
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    • 2019
  • An analytical method was developed for the determination of broflanilide and its metabolites in agricultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with acetonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl ($C_{18}$). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative standard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effective and sensitive for broflanilide determination in agricultural commodities.

Studies on the physio-chemical properties and the cultivation of oyster mushroom(Pleurotus ostreatus) (느타리버섯의 생리화학적성질(生理化學的性質) 및 재배(栽培)에 관(關)한 연구(硏究))

  • Hong, Jai-Sik
    • Applied Biological Chemistry
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    • v.21 no.3
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    • pp.150-184
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    • 1978
  • Nutritional characteristics and physio-chemical properties of mycelial growth and fruitbody formation of oyster mushroom(Pleurotus ostreatus)in synthetic media, the curtural condition for the commerical production in the rice straw and poplar sawdust media, and the changes of the chemical components of the media and mushroom during the cultivation were investigated. The results can be summarized as follows: 1. Among the carbon sources mannitol and sucrose gave rapid mycelial growth and rapid formation of fruit-body with higher yield, while lactose and rhamnose gave no mycelial growth. Also, citric acid, succinic acid, ethyl alcohol and glycerol gave poor fruit-body formation, and acetic acid, formic acid, fumaric acid, n-butyl alcohol, n-propyl alcohol and iso-butyl alcohol inhibited mycelial growth. 2. Among the nitrogen sources peptone gave rapid mycelial growth and rapid formation of fruit-body with higher yield, while D,L-alanine, asparatic acid, glycine and serine gave very poor fruit-body formation, and nitrite nitrogens, L-tryptophan and L-tyrosine inhibited mycelial growth. Inorganic nitrogens and amino acids added to peptone were effective for fruit-body growth, and thus addition of ammonium sulfate, ammonium tartarate, D,L-alanine and L-leucine resulted in about 10% increase fruit-body yield. L-asparic acid about 15%, L-arginine about 20%, L-glutamic acid, and L-lysine about 25%. 3. At C/N ratio of 15.23 fruit-body formation was fast, but the yield decreased, and at C/N ratio of 11.42 fruit-body formation was slow, but the yield increased. Also, at the same C/N ratio the higher the concentration of mannitol and petone, the higher yield was produced. Thus, from the view point of both yield of fruit-body and time required for fruiting the optimum C/N ratio would be 30. 46. 4. Thiamine, potassium dihydrogen phosphate and magnecium sulfate at the concentration of $50{\mu}g%$. 0.2% and 0.02-0.03%, respectively, gave excellent mycelial and fruit-body growth. Among the micronutrients ferrous sulfate, zinc sulfate and manganese sulfate showed synergetic growth promoting effect but lack of manganese resulted in a little reduction in mycelial and fruit-body growth. The optimum concentrati on of each these nutrients was 0.02mg%. 5. Cytosine and indole acetic acid at 0.2-1mg% and 0.01mg%, respectively, increased amount of mycelia, but had no effect on yield of fruit-body. The other purine and pyrimidine bases and plant hormones also had no effect on mycelial and fruit-belly yield. 6. Illumination inhibited mycelial growth, but illumination during the latter part of vegetative growth induced primordia formation. The optimum light intensity and exposure time was 100 to 500 lux and 6-12 hours per day, respectively. Higher intensity of light was injurous, and in darkness only vegetative growth without primordia formation was continued. 7. The optimum temperature for mycelial growth was $25^{\circ}C$ and for fruit-body formation 10 to $15^{\circi}C$. The optimum pH range was from 5.0 to 6.5. The most excellent fry it-body formation were produced from the mycelium grown for 7 to 10 days. The lesser the volume of media, the more rapid the formation of fruit-body; and the lower the yield of fruit-body; and the more the volume of media, the slower the formation of fruit-body, and the higher the yield of fruit-body. The primordia formation was inhibited by $CO_2$. 8. The optimum moisture content for mycelial growth was over 70% in the bottle media of rice straw and poplar sawdust. 10% addition of rice bran to the media exhibited excellent mycelial growth and fruit-body formation, and the addition of calciumcarbonate alone was effective, but the addition of calcium carbonate was ineffective in the presence of rice bran. 9. In the cultivation experiments the total yield of mushroom from the rice straw media was $14.99kg/m^2$, and from the sawdust media $6.52kg/m^2$, 90% of which was produced from the first and second cropping period. The total yield from the rice straw media was about 2.3 times as high as that from the sawdust media. 10. Among the chemical components of the media little change was observed in the content of ash on the dry weight basis, and organic matter content decreased as the cultivation progressed. Moisture content, which was about 79% at the time of spawning, decreased a little during the period of mycelial propagation, after which no change was observed. 11. During the period from spawning to the fourth cropping about 16.7% of the dry matter, about 19.3% of organic matter, and about 40% of nitrogen were lost from the rice straw media; about 7.5% of dry mallet, about 7.6% of organic matter, and about 20% of nitrogen were lost from the sawdust media. For the production of 1kg of mushroom about 232g of organic matter and about 7.0g of nitrogen were consumed from the rice straw media; about 235g of organic matter and about 6.8g of nitrogen were consumed from the sawdust media, 1㎏ of mushroom from either of media contains 82.4 and 82.3g of organic matter and 5.6 and 5.4g of nitrogen, respectively. 12. Total nitrogen content of the two media decreased gradually as the cultivation progressed, and total loss of insoluble nitrogen was greater than that of soluble nitrogen. Content of amino nitrogen continued to increase up to the third cropping time, after which it decreased. 13. In the rice straw media 28.0 and 13.8% of the total pentosan and ${\alpha}$-cellulose, respectively, lost during the whole cultivation period was lost during the period of mycelial growth; in the sawdust media 24.1 and 11.9% of the total pentosan and ${\alpha}$-cellulose, respectively, was lost during the period of mycelial growth. Lignin content in the media began to decrease slightly from the second cropping time, while the content of reduced sugar, trehalose and mannitol continued to increase. C/N ratio of the rice straw media decreased from 33.2 at spawining to 30.0 at ending; that of the sawdust media decreased from 61.3 to 60.0. 14. In both media phosphorus, potassium, manganese and zinc decreased, at magnesium, calcium and copper showed irregular changes, and iron had a tendency to be increased. 15. Enzyme activities are much higher in the rice straw media than in the sawdust media. CMC saccharifying and liquefying activity gradually increased from after mycelial propagation to the second cropping, after which it decreased in both media. Xylanase activity rapidly and greatly increased during the second cropping period rather than the first period. At the start of the third cropping period the activity decreased rapidly in the rice straw media, which was not observed in the sawdust media. Protease activity was highest after mycelial propagation, after which it gradually decreased. The pH of the rice straw media decreased from 6.3 at spawning to 5.0 after fourth cropping; that of the sawdust media decreased from 5.7 to 4.9. 16. The contents of all the components except crude fibre of the mushroom from the rice straw media were higher than those from the sawdust media. Little change was observed in the content of the components of mushroom cropped from the first to the third period, but slight decrease was noticed at the fourth cropping.

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The Chemical Composition of the Nagdong River Downstream Water (낙동강 하류수의 수질조성에 대하여)

  • WON Jong Hun;LEE Bae Jung
    • Korean Journal of Fisheries and Aquatic Sciences
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    • v.14 no.2
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    • pp.47-58
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    • 1981
  • Relationships between the electrical conductivity and the contents of the chloride, sulfate, calcium, magnesium, sodium, potassium and total major inorganic ions, and between each, chemical conservative constituents were calculated with the data which sampled at the lesions of Mulgeum and between Namji and Wondong from March 1974 to April 1980. Semilogarithmic relations were found between the electrical conductivity and the contents of monovalent ions, and logarithmic relations were found between the electrical conductivity and the contents of divalent ions at the both regions. The relational equations between the electrical conductivity $\lambda_{25}$and the contents of the major inorganic ions at Mulgeum are as follows: $log\;Cl(ppm)\;=\;2.37{\cdot}\lambda_{25}(m{\mho}/cm)+0.733{\pm}0.141$, $log\;SO_4(ppm)=1.12{\cdot}log\lambda_{25}(m{\mho}/cm)+2.14{\pm}0.18$, $log\;Ca(ppm)=0.615{\cdot}log\lambda_{25}(m{\mho}/cm)+1.67{\pm}0.12$, $log\;Mg(ppm)=0.756{\cdot}log\lambda_{25}(m{\mho}/cm)+1.27{\pm}0.11$, $log\;Na(ppm)=2.82{\cdot}\lambda_{25}(m{\mho}/cm)+0.551{\pm}0.133$, $log\;K(ppm)=1.33{\cdot}\lambda_{25}(m{\mho}/cm)+0.136{\pm}0.095$, and total inorganic ions $C(ppm)=399{\cdot}\lambda_{25}(m{\mho}/cm)-0.9{\pm}14.6$. The relational equations between the electrical conductivity ($\lambda_{25}$) and the contents of the major inorganic ions at the region between Namji and Wondong a.e as follows: $log\;Cl(ppm)=4.27{\cdot}\lambda_{25}(m{\mho}/cm)+0.380{\pm}0.138$, $log\;SO_4(ppm)=0.915{\cdot}log\lambda_{25}(m{\mho}/cm)+1.95{\pm}0.18$, $log\;Ca(ppm)=0.756{\cdot}log\lambda_{25}(m{\mho}/cm)+1.74{\pm}0.12$, $log\;Mg(ppm)=1.00{\cdot}log\lambda_{25}(m{\mho}/cm)+1.41{\pm}0.10$. $log\;Na(ppm)=2.47{\cdot}\lambda_{25}(m{\mho}/cm)+0.614{\pm}0.065$, $log\;K(ppm)=1.62{\cdot}\lambda_{25}(m{\mho}/cm)+0.030{\pm}0.060$, and total inorganic ions $C(ppm)=323{\cdot}\lambda_{25}(m{\mho}/cm)+11.7{\pm}9.3$. Logarithmic relations were found between each chemical conservative constituents at Mulgeum and the equations are as follows: $log\;Cl(ppm)=0.711{\cdot}log\;SO_4(ppm)+0.488{\pm}0.206$, $log\;Cl(ppm)=0.337{\cdot}log\;Ca(ppm)+0.822{\pm}0.130$, $log\;Cl(ppm)=0.605{\cdot}log\;Mg(ppm)-0.017{\pm}0.154$, $Cl(ppm)=0.676{\cdot}Na(ppm)+2.31{\pm}4.67$, $log\;Cl(ppm)=0.406{\cdot}log\;K(ppm)-0.092{\pm}0.112$, $log\;SO_4(ppm)=0.378{\cdot}log\;Ca(ppm)+0.721{\pm}0.125$, $log\;SO_4(ppm)=0.462{\cdot}log\;Mg(ppm)+0.107{\pm}0.118$, $log\;SO_4(ppm)=0.592{\cdot}log\;Na(ppm)+0.313{\pm}0.191$, $log\;SO_4(ppm)=0.308{\cdot}log\;K(ppm)-0.019{\pm}0.120$, $Ca(ppm)=0.262{\cdot}Mg(ppm)+0.74{\pm}1.71$. $log\;Ca(ppm)=1.10{\cdot}log\;Na(ppm)-0.243{\pm}0.239$, $Ca(ppm)=0.0737{\cdot}K(ppm)+1.26{\pm}0.73$, $log\;Mg(ppm)=0.0950{\cdot}Na(ppm)+0.587{\pm}0.159$, $log\;Mg(ppm)=0.0518{\cdot}K(ppm)+0.111{\pm}0.102$, and $Na(ppm)=0.0771{\cdot}K(ppm)+1.49{\pm}0.59$. Logarithmic relations were found between each chemical conservative constituents except a relationship between the chloride and calcium contents at the region between Namji and Wondong, and the equations are as follows : $log\;Cl(ppm)=0.312{\cdot}log\;SO_4(ppm)+0.907{\pm}0.210$, $log\;Cl(ppm)=0.458{\cdot}log\;Mg(ppm)+0.135{\pm}0.130$, $Cl(ppm)=0.484{\cdot}logNa(ppm)+0.507{\pm}0.081$, $Cl(ppm)=0.0476{\cdot}K(ppm)+1.41{\pm}0.34$, $log\;SO_4(ppm)=0.886{\cdot}log\;Ca(ppm)+0.046{\pm}0.050$, $log\;SO_4(ppm)=0.422{\cdot}log\;Mg(ppm)+0.139{\pm}0.161$, $log\;SO_4(ppm)=0.374{\cdot}log\;Na(ppm)+0.603{\pm}0.140$, $log\;SO_4(ppm)=0.245{\cdot}log\;K(ppm)+0.023{\pm}0.102$, $log\;Ca(ppm)=0.587{\cdot}log\;Mg(ppm)+0.003{\pm}0.088$, $log\;Ca(ppm)=0.892{\cdot}log\;Na(ppm)+0.028{\pm}0.109$, $log\;Ca(ppm)=0.294{\cdot}log\;K(ppm)-0.001{\pm}0.085$, $log\;Mg(ppm)=0.600{\cdot}log\;Na(ppm)+0.674{\pm}0.120$, $log\;Mg(ppm)=0.440{\cdot}log\;K(ppm)+0.038{\pm}0.081$, and $log\;Na(ppm)=0.522{\cdot}log\;K(ppm)-0.260{\pm}0.072$.

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