• Title/Summary/Keyword: liquid standard

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A Study on the Simultaneous Determination of Residual Zeranol, Zearalenone and Their Metabolites in Beef by Gas Chromatography/Mass Spectrometry (Gas Chromatography/Mass Spectrometry에 의한 우육 중의 잔류 Zeranol, Zearalenone 및 그 대사산물들의 동시 분석법에 대한 연구)

  • 이은섭;이용욱
    • Journal of Food Hygiene and Safety
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    • v.9 no.1
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    • pp.1-13
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    • 1994
  • A Simultaneous determination method was improved for the determination and confirmation of zeranol, zearalenone, as well as their isomers and metabolites, in beef. The analytes were extracted from tissue by CH3CN, hydrolyzed enzymatically(for glucuronide conjugates), cleaned up by a strong basic anion exchange resin combined with a liquid/liquid partitioning, derivatized using MSTFA and confirmed, quantified by GC/MS/SIM with a internal standard, zearalane. The results were as follows : (1) all the estrogens were separated on the GC/MS chromatogram under the extraction method and the chromatographic conditions improved, the retention times of zearalane-TMS2, zearalanone-TMS2, zearalenone-TMS2, zeranol-TMS3, taleranol-TMS3, and $\alpha$-zearalenol-TMS3, $\beta$-zearalenol-TMS3, were 18.49, 19.44, 19.63, 19.71, 19.79 and 19.99, 20.08 minutes, respectively. (2) The calibration curves of residual zeranol, zearalenone and their metabolites showed constantly linear(r=0.99) in the range of 5~20 ng. The minimum detection concentration of residual zeranol, zearalenone and their metabolites was 1 ppb. (3) The total average recovery of residual zeranol, zearalenone and their metabolites from spiked beef was 60.2%(CV=29.7%) at the 1 ppb and 63.5%(CV=26.5) at the 2 ppb, 72.9%(CV=18.2%) at the 4 ppb. (4) The preservation method for 6 estrogens was improved for the fast running time(21 min) and MSTFA was utilized for derivatizing 6 estrogens for improvement of recovery, for good resolution, for characteristic mass spectra unlike Jose's method and Tina's method. The utilization of zearalane as internal standard showed good quantification result for zeranol, zearalenone, as well as their isomers and metabolites, in beef.

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Studies on Analysis of Food Additives (II). Determination of Nitrite by High Performance Liquid Chromatography (식품첨가물의 분석에 관한 연구(II) 고속액체 크로마토그라피에 의한 아질산의 정량)

  • 천석조;임영희;송인상;노정배
    • Journal of Food Hygiene and Safety
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    • v.3 no.3
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    • pp.99-103
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    • 1988
  • For the purpose of discussing two colorimetric methods modified from the Standard Methods of Sanitary Inspection. Guide issued by the Ministry of Health and Social Affaires of Korea (1985), the Standard Methods of Analysis of Hygienic Chemists authorized by the Pharmaceutical Society of Japan.(1980) and HPLC (high performance liquid chromatography) method were studied. Two kinds of ham, sausage samples and four kinds of roe samples were analyzed by the HPLC method and the results agreed well with those obtained by the diazotization-coupling colorimetric method prescribed in the Standard Methods of Analysis for Hygienic Chemists authorized by the Pharmaceutical Society of Japan (1980) and two modified methods.

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The effect of relative humidity on the performance of DNPH-cartridge sampling for odorous aldehydes (악취성 Carbonyl 화합물의 카트리지 채취 분석: 습도가 채취효율에 미치는 영향)

  • Lee, Min-Hee;Kim, Ki-Hyun
    • Analytical Science and Technology
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    • v.25 no.1
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    • pp.50-59
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    • 2012
  • In this study, the effect of humidity change on DNPH cartridge sampling efficiency for carbonyl compounds (CCs) has been investigated. For this analysis, gaseous standard of 6 different CCs (formaldehyde (FA), acetaldehyde (AA), propionaldehyde (PA), butyraldehyde (BA), isovaleraldehyde (IA), and valeraldehyde (VA)) was calibrated after derivatization with three types of DNPH cartridge products. Their calibration results derived at RH values between 0 and 80% were then compared against liquid phase standards. If the results of our analysis are compared by the RH values between 20 and 80%, the effect of RH can be distinguished between light and heavy CCs. For lighter CCs (like FA and AA), there was no significant change. However, for the ones heavier than PA, there was fairly noticeable increase in relative recovery ratio in RH value between 20 and 80%. Such patterns are seen consistently from all three DNPH products tested for comparison. The results of our analysis suggest that proper correction for RH change may be needed for heavier CCs by the cartridge method.

Evaluation of Matrix Effects in Quantifying Microbial Secondary Metabolites in Indoor Dust Using Ultraperformance Liquid Chromatographe-Tandem Mass Spectrometer

  • Jaderson, Mukhtar;Park, Ju-Hyeong
    • Safety and Health at Work
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    • v.10 no.2
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    • pp.196-204
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    • 2019
  • Background: Liquid chromatography-tandem mass spectrometry (LC-MSMS) for simultaneous analysis of multiple microbial secondary metabolites (MSMs) is potentially subject to interference by matrix components. Methods: We examined potential matrix effects (MEs) in analyses of 31 MSMs using ultraperformance LC-MSMS. Twenty-one dust aliquots from three buildings (seven aliquots/building) were spiked with seven concentrations of each of the MSMs ($6.2pg/{\mu}l-900pg/{\mu}l$) and then extracted. Another set of 21 aliquots were first extracted and then, the extract was spiked with the same concentrations. We added deepoxy-deoxynivalenol (DOM) to all aliquots as a universal internal standard. Ten microliters of the extract was injected into the ultraperformance LC-MSMS. ME was calculated by subtracting the percentage of the response of analyte in spiked extract to that in neat standard from 100. Spiked extract results were used to create a matrix-matched calibration (MMC) curve for estimating MSM concentration in dust spiked before extraction. Results: Analysis of variance was used to examine effects of compound (MSM), building and concentration on response. MEs (range: 63.4%-99.97%) significantly differed by MSM (p < 0.01) and building (p < 0.05). Mean percent recoveries adjusted with DOM and the MMC method were 246.3% (SD = 226.0) and 86.3% (SD = 70.7), respectively. Conclusion: We found that dust MEs resulted in substantial underestimation in quantifying MSMs and that DOM was not an optimal universal internal standard for the adjustment but that the MMC method resulted in more accurate and precise recovery compared with DOM. More research on adjustment methods for dust MEs in the simultaneous analyses of multiple MSMs using LC-MSMS is warranted.

Elution Behavior of Pd(II) - Isonitrosoethylacetoacetate Imine Chelates by Reversed Phase High Performance liquid Chromatography (역상 액체 크로마토그래피에 의한 Pd(II) - Isonitrosoethylacetoacetate Imine 유도체 킬레이트들의 용리 거동)

  • Kim, In-Whan;Shin, Han-Chul;Lee, Man-Ho;Yoon, Tai-Kun;Kang, Chang-Hee;Lee, Won
    • Analytical Science and Technology
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    • v.5 no.4
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    • pp.389-399
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    • 1992
  • Liquid Chromatographic behavior of Pd(II) in Isonitrosoethylacetoacetate lmine, $Pd(IEAA-NR)_2$ (R=H, $CH_3$, $C_2H_5$, $n-C_3H_7$, $C_6H_5-CH_2$, $n-C_4H_9$) chelates were investigated by reversed-phase HPLC on Micropak MCH-5 column using methanol/water as mobile phase. The optimum conditions for the separation of $Pd(IEAA-NR)_2$ chelates were examined with respect to the effect of the flow rate, sample solvent, mobile phase strength and column temperature. It wass found that metal chelates were properly eluted in an acceptable range of capacity factor value($0{\leq}log\;k^{\prime}{\leq}1$). The dependence of the logarithm of capacity factor(k') on the volume fraction of water in the binary mobile phase was examined. Also, the dependence of k' on the liquid-liquid extration distribution ratio($D_c$) in methanol-water/n-alkane extration system was investigated. Both kinds of dependence are linear, which susggests that the retention of the electroneutral metal chelate is largely due to the solvophobic effect. Standard adsorption enthalpy changes (${\Delta}H^{\circ}$) and standard adsorption entropy changes (${\Delta}S^{\circ}$) of Pd(II) Isonitrosoethylacetoacetate imine chelates on Micropak MCH-5 column were calculated by measuring capacity factor with changing temperature of the column.

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Study on Phosphorus Removal in the Secondary Effluent by Flotation Using Microbubble Liquid Film System (미세기포 액막화 부상법을 이용한 하수 2차 처리수의 인 제거에 관한 연구)

  • Lee, Shun-Hwa;Kang, Hyun-Woo;Lee, Se-Han;Kwon, Jin-Ha;Jung, Kye-Joo
    • Journal of Korean Society of Environmental Engineers
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    • v.34 no.1
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    • pp.42-48
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    • 2012
  • In this study, experiment on phosphorus removal was performed by using microbubble liquid film flotation tank with microbubble module. After dissolving gas and liquid in dissolving tank, microbubble liquid film system created microbubbles in equal size under fixed low pressure. After being passed through $A_2O$ and m-$O_3$ process, secondary treatment wastewater was used as influent in phosphorus removal process. When the T-P concentration of influent was 2.89 mg/L, alum(8%, 30 mg/L) was injected into a microbubble flotation tank, the treatment resulted 94% of T-P removal rate. Remaining T-P concentration was less than 0.2 mg/L, which is in accord with the effluent quality standard. Seasonal variations in water temperature showed no differences in T-P removal property. When the inflow concentration of SS was 1.0 mg/L or more, it served as coagulation nuclei in the coagulation process. In that condition, average T-P removal rate was higher than 97%. When 50% of floated scum was returned, coagulator Al included in scum assisted the injected coagulator and maximized the coagulation efficiency of pollutant. In such treatment, the T-P concentration was measured as 0.18 mg/L and satisfied the outflow water quality standard, which is 0.2 mg/L or less.

Nutrient Composition and Heavy Metal Contents of Matured Livestock Liquid Fertilizer in Korea (국내 가축분뇨 부숙액비의 비료성분 및 중금속 함량 분포특성)

  • Kang, Tak-Won;Halder, Joshua Nizel;Kim, Soo-Ryang;Yoon, Young-Man;Lee, Myung-Gyu
    • Journal of the Korea Organic Resources Recycling Association
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    • v.25 no.4
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    • pp.31-39
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    • 2017
  • From July to August 2013, liquid fertilizers produced at 180 liquid manure public resource centers and liquid fertilizer distribution centers were collected. The maturity of liquid fertilizers was measured using the mechanical maturity measurement device. The nutrient contents (nitrogen, phosphorus, and potassium), physicochemical properties, and heavy metal content of 46 liquid fertilizers were investigated in this study. We used a matured liquid fertilizer with a total number of 46, with number of 7 for Gyeonggi-do, 3 for Chungcheongbuk-do, 2 for Chungcheongnam-do, 13 for Jeollabuk-do, 5 for Jeollanam-do, 3 for Gyeongsangbuk-do, 11 for Gyeongsangnam-do, 1 for Daejeon, and 1 for Jeju-do. The physicochemical properties were as follows: pH 8.0, EC 11.6 mS/cm, SS 5,188 mg/L, TKN 847mg/L, ${{NH_4}^+}-N$ 317 mg/L, ${{NO_3}^-}-N$ 170 mg/L, Org-N 360 mg/L, TP 193 mg/L, and TK 2,557 mg/L. The total amount of NPK was 3,596 mg/L. The total amount of N-P-K was as follows: a number of 2 at 1,000-2,000 mg/L (4%), a number of 17 at 2,000-3,000mg/L (37%), a number of 11 at 3,000-4,000mg/L (24%), and a number of 16 at 4,000mg/L or more (35%). Thus, 41% of the mature liquid fertilizers were below the official standard of commercial fertilizer (livestock manure liquid fertilizer) (0.3% of the total amount of N-P-K). Most of the N-P-K total amount showed non-uniform characteristics of low nitrogen and low phosphoric acid due to the potassium concentration. The average heavy metal content in the matured liquid fertilizer was as follows: As, not detected; Cd, 0.01 mg/kg; Hg, not detected; Pb, 0.02 mg/kg; Cr, 0.14 mg/kg; Cu, 6.89 mg/kg; Ni, 0.44 mg/kg; and Zn, 20.70 mg/kg. Thus, the official standard of commercial fertilizer was satisfied in all categories, indicating a safe level.

The Effect of Digestive Medicine on Enamel Erosion (액상소화제가 법랑질 부식에 미치는 영향)

  • Lee, Hye-Jin;Oh, Han-Na
    • Journal of dental hygiene science
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    • v.17 no.4
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    • pp.352-357
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    • 2017
  • Consumption of liquid digestive medicine has continually grown in recent years. This present study was designed to evaluate the capability of liquid digestive medicine to erode dental enamel, relating the pH and titratable acidity of liquid digestive medicine. Three commercially available liquid digestive medicines were chosen these were Gashwalmyeungsu, Saengrokchun and Wicheongsu. The liquid digestive medicines were evaluated in respect to pH, titratable acidity and concentrations of calcium and phosphate, respectively. This measure was carried out three times for each digestive medicine and was recorded the data as mean (standard deviation). Bovine enamel specimens measured microhardness at base line and then were randomly assigned to 4 groups of 10 each. The specimens were immersed into each liquid digestive medicine for 1, 3, 5, 10, 15, and 30 minutes and then evaluated each time by VHN. All digestive medicines had a pH of less than 3.7. Wicheongsu had the lowest pH 2.93 and Gashwalmyeungsu had highest pH 3.63. In pH 5.5, titratable acidity of Wicheongsu was 1.27 ml. Gashwalmyeungsu was 0.63 ml. Saengrokchun was 0.60 ml. All liquid digestive medicines showed low concentration of calcium and phosphate. The microhardness of specimens after immersion into liquid digestive medicines was continuously reduced in all digestive medicines. After 30-minute treatment in liquid digestive medicines, Wicheongsu containing low pH and high tiratable acidity was shown to be lowest microhardness value ($207.80{\pm}15.52$). The three liquid digestive medicines caused surface softening of enamel erosion. We conclude that drinks, commonly consumed by functional dyspepsia patient can cause erosion of enamel.

In situ UHV TEM studies on nanobubbles in graphene liquid cells

  • Shin, Dongha;Park, Jong Bo;Kim, Yong-Jin;Kim, Sang Jin;Kang, Jin Hyoun;Lee, Bora;Cho, Sung-Pyo;Novoselov, Konstantin S.;Hong, Byung Hee
    • Proceedings of the Korean Vacuum Society Conference
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    • 2016.02a
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    • pp.102-102
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    • 2016
  • Water, which is most abundant in Earth surface and very closely related to all forms of living organisms, has a simple molecular structure but exhibits very unique physical and chemical properties. Even though tremendous effort has been paid to understand this nature's core substance, there amazingly still lefts much room for scientist to explore its novel behaviors. Especially, as the scale goes down to nano-regime, water shows extraordinary properties that are not observable in bulk state. One of such interesting features is the formation of nanoscale bubbles showing unusual long-term stability. Nanobubbles can be spontaneously formed in water on hydrophobic surface or by decompression of gas-saturated liquid. In addition, the nanobubbles can be generated during electrochemical reaction at normal hydrogen electrode (NHE), which possibly distorts the standard reduction potential at NHE as the surface nanobubble screens the reaction with electrolyte solution. However, the real-time evolution of these nanobubbles has been hardly studied owing to the lack of proper imaging tools in liquid phase at nanoscale. Here we demonstrate, for the first time, that the behaviors of nanobubbles can be visualized by in situ transmission electron microscope (TEM), utilizing graphene as liquid cell membrane. The results indicate that there is a critical radius that determines the long-term stability of nanobubbles. In addition, we find two different pathways of nanobubble growth: i) Ostwald ripening of large and small nanobubbles and ii) coalescence of similar-sized nanobubbles. We also observe that the nucleation and growth of nanoparticles and the self-assembly of biomolecules are catalyzed at the nanobubble interface. Our finding is expected to provide a deeper insight to understand unusual chemical, biological and environmental phenomena where nanoscale gas-state is involved.

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Study on Leakage Measurements of Oxygen and Helium Using Standard Gas Flow Rates in a Orifice Flow (오리피스에서 기체의 표준유량을 이용한 산소와 헬륨의 누설량 측정에 관한 연구)

  • Lee, Joongyoup;Han, Sangyeop;Huh, Hwanil
    • Journal of the Korean Society for Aeronautical & Space Sciences
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    • v.43 no.12
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    • pp.1108-1115
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    • 2015
  • In this study, correlation equations were arranged about mass flow rates of oxygen and volume flow rates of helium using a mouthpiece method. The mouthpiece method can reduce examination cost by using similar empirical formula. Instead of liquid oxygen, in the mouthpiece method, gas helium can be measured in order to determine the leakage amount of liquid oxygen conveniently. Experiment was conducted and compared to understand leakage amount relation between the helium and the oxygen for prototype item under a room and a cryogenic temperature conditions. The leakage volume flow rate [$A.m{\ell}/s$] of the helium was 174 times higher than mass flow rate [g/s] of the oxygen leakage at liquid state. The derived correlation equations were verified using data from the National Institute of Standards and Technology (NIST).