• Title/Summary/Keyword: 70% ACN

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Determination of tylosin in edible meats by high-performance liquid chromatography (HPLC를 이용한 식육내 타이로신의 잔류분석법)

  • Kim, Gon-sup;Shin, Sun-hye;Kim, Jong-su;Ra, Do-kyung
    • Korean Journal of Veterinary Research
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    • v.41 no.1
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    • pp.13-19
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    • 2001
  • A simple and rapid analytical method for the determination of tylosin in chicken, pork and muscle was established by High-Performance Liquid Chromatography(HPLC). Chicken, pork and beef muscle(5 g) were fortified by adding the $0.2{\mu}g/ml$ of standard tylosin and the drug was extracted from meats with 70% acetonitrile(ACN) and followed by liquid-liquid partition for clean-up procedure. Then $20{\mu}l$ portion of ACN elution was directly analyzed by HPLC with spectra 100 variable wavelength detector, and unfortified blank control were treated similarly. The average recovery rate of tylosin added to chicken, pork and beef muscle were $83{\pm}2.3$, $96{\pm}3.3$ and $92{\pm}1.6$(%) at the level 0.2 ppm, respectively. No tylosin residues in marketing meats. These results suggested that HPLC methodology could be acceptable for the extraction, determination and screening of tylosin residues in edible meats.

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Determination of Aldehydes in Tap Water by Reverse Phase Liquid Chromatography (역상 액체 크로마토그래피에 의한 수도수 중 알데하이드류의 정량)

  • Choi, Yong Wook;Choi, Yun Jung
    • Journal of the Korean Chemical Society
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    • v.43 no.4
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    • pp.438-446
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    • 1999
  • The optimum analytical method of aldehydes, ozone by-products, was established by reverse phase liquid chromatography. Six aldehydes including formaldehyde, acetaldehyde, acrolein, propionaldehyde, butylaldehyde and benzaldehyde, and one ketone including acetone were selected as aldehyde test samples through preliminary experiments. Such analytical conditions as the pH of citrate buffer solution, reaction temperature, reaction time, and concentration of DNPH, the component and composition of desorption solvent were optimized. As the result, pH 3.0 of citrate buffer solution, 40$^{\circ}C$ of reaction temperature, 15 minutes of reaction time, and 0.012% of DNPH concentration were chosen as optimum conditions. Aldehydes-DNPH derivatives in water were concentrated on $C_18$ Sep-Pak cartridge and followed by elution of their derivatives fraction with THF/ACN(70/30) mixture, and showed recoveries of the range from 87 to 107%. Separation condition on Nova-Pak $C_18$ column with low pressure gradient elution from ACN/MeOH/water(30/10/60) of an initial condition to 80% ACN of a final condition was found to give a good resolution within 20 minutes of run time. 86% to 103% of recovery for aldehydes using this method was similar to that for aldehyde using EPA Method 554 which is ranged from 84% to 103%.

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Separation of Egg White Using HPLC with Change of Mobile Phase and Temperature (HPLC에서 이동상 변화와 온도에 따른 난백의 분리)

  • Do, Jin-Sun;Song, Shin-Young;Cho, Ki-Jung;Kim, In-Ho
    • Korean Chemical Engineering Research
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    • v.49 no.6
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    • pp.829-834
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    • 2011
  • Lysozyme in egg white functions as bacteriolysis agent and ovalbumin plays a role as antigen in immune system. Egg white analysis methods usually include electrophoresis, gel permeation chromatography and reversed-phase HPLC(RP-HPLC). Among them, RP-HPLC was selected for rapid analysis and C18 column(Agilent, USA) was used as HPLC column. Optimum conditions were searched by changing mobile phase and temperature. Capacity factor and resolution were calculated and compared for various elution conditions. In the isocratic elution, mobile phase volume ratio was changed from 30/70/0.1 to 60/40/0.1(Acetonitrile(ACN)/Distilled water(DW)/Trifluoroacetic acid(TFA)). ACN composition was increased by 10% and temperature was set as $20^{\circ}C$. In the gradient elution, ACN/DW ratio was changed from 10/90 to 60/40 during 20 minute and temperature was varied as 20, 30 and $40^{\circ}C$. In the isocratic elution, three peaks were separated at 50/50/0.1. Lysozyme and ovalbumin were confirmed as first and third peak in three peaks respectively. In the gradient elution, four peaks were separated at $30^{\circ}C$. Lysozyme and ovalbumin were confirmed as first peak and third peak in four peaks respectively.

Effects of Temperature and Acetonitrile on Microwave-Assisted Weak Acid Protein Hydrolysis

  • Nam, Mihyeon;Lee, Dabin;Kim, Yeoseon;Kim, Jeongkwon
    • Mass Spectrometry Letters
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    • v.9 no.2
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    • pp.46-50
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    • 2018
  • The effects of temperature and acetonitrile (ACN) concentration on microwave-assisted weak-acid hydrolysis of proteins were investigated. Myoglobin was hydrolyzed for 1 h using 2% formic acid and a microwave with different concentrations of ACN (0, 5, and 10%) at various temperatures (50, 60, 70, 80, 90, and $100^{\circ}C$). The numbers of peptides identified with each concentration of ACN were the same for each temperature. The greatest number of peptides (18 total) was obtained with hydrolysis at $100^{\circ}C$, and 6 of these were a result of additional removal of aspartic acid at the C-terminus. Hydrolysis at $80^{\circ}C$ resulted in 13 peptides, of which only 1 was generated by the additional removal of aspartic acid, and 12 were observed with hydrolysis at $100^{\circ}C$. Our results demonstrate that microwave-assisted weak-acid hydrolysis of proteins can be performed successfully at $80^{\circ}C$, which could be beneficial for limiting side reactions and generating larger peptide sequences.

A Comparison of Sampling and Analytical Methods for Airborne Isocyanates (공기중 이소시아네이트류의 측정 및 분석방법에 관한 비교연구)

  • 변혜정;윤충식;백남원
    • Journal of Environmental Health Sciences
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    • v.22 no.2
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    • pp.32-42
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    • 1996
  • This study was performed to evaluate accuracy and precision of filter method and impinger method for analyzin airborne isocyanates in mixture (2, 6-TDI, HDI, 2, 4-TDI, MDI). Filter method was performed using the OSHA Method 42 and impinger method using the NIOSH Method 5521. The samples were analyzed by high performance liquid chromatography-ultraviolet detector (HPLC-UVD). After the optimum operating conditions for each method were investigated, samples with various concentration levels were quantified at the conditions. The precision was expressed by the pooled coefficient of variation(C.V.) and the accuracy by overall accuracy. The results are summarized as follows: 1. The optimum condition of filter method was determined at 35/65 ACN/buffer (0.01 M ammonium acetate) in mobile phase. And in case of impinger method, it was at 30/70 ACN/buffer(0.2 M sodium acetate). The effect of concentrations of acetate on the separation of the peaks was not significant, but, the effect of ACN/buffer ratio was significant. 2. The correlation coefficients for the two methods were above 0.9 in all isocyanate compounds. Average recovery efficiencies for 2, 6-TDI, HDI, 2, 4-TDI and MDI in filter method were 92.4%, 102.6%, 87.3% and 101.0%, respectively. Those in impinger method were 106.6%, 106.7%, 99.0% and 103.6%, respectively. As a result, the recovery efficiency of impinger method was higher than those of filter method in analyzing isocyanate compounds. 3. The pooled coefficients of variations of the methods were slightly higher than expected. The overall accuracies of the methods were within $\pm 25%$ for each isocyanate compound. Since these results satisfy NIOSH criteria, the accuracy of the experiment is appropriate. 4. As seen above, impinger method is more efficient than filter method. But, there are many disadvantages in impinger method. Therefore, solid sorbent such as a glass fiber filter must be developed in order to have the high efficiency not less than that of impinger method in the future.

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Discrimination of Domestic Rice Cultivars by Capillary Electrophoresis (Capillary Electrophoresis를 이용한 국내산 쌀의 품종 판별)

  • Rhyu, Mee-Ra;Kim, Eun-Young;Ahn, Mee-Ok;Kim, Sang-Sook
    • Korean Journal of Food Science and Technology
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    • v.30 no.6
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    • pp.1252-1258
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    • 1998
  • Capillary electrophoresis (CE) with rice proteins was used to discriminate 10 domestic rice cultivars in less than 25 min. Most cultivars were differentiated quickly and easily using P-ACN buffer system. CE of rice prolamins allowed classifying ten varieties of Korean rice into three groups. Peak h was characteristic peak for Dongjinbyeo, Gaehwabyeo and Yongnambyeo which were classified into the group of Dongjinbyeo. Chuchungbyeo, Odaebyeo, Mangeumbyeo and Bonggwangbyeo easily differentiated from the group of Dongjinbyeo by the absence of peak h which were classified into the group of Chuchungbyeo. Peak g typical for Illpumbyeo, Hwaseungbyeo and Hwayoungbyeo accounted for 70% of total peak area. They belong to the group of Illpumbyeo. Some cultivars showed specific peak patterns among ten cultivars, Illpumbyeo was differentiated from others by several peaks between peak c and peak f, and the peak d was apparently detected in Odaebyeo not in others. Other minor differences were also found within each group. The result of the study showed that CE has potential for discrimination of rice cultivars. It also possesses the inherent advantages such as low mass requirements, fast seperations, and quantitative analysis through on-capillary UV detection.

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Simultaneous Determination of Isocyanates by High Performance Liquid Chromatography (고속액체크로마토그래피를 이용한 이소시아네이트의 동시 정량)

  • Lee, Seon Joo;Lee, Kwang Mook;Roh, Young Man
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.4 no.2
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    • pp.137-147
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    • 1994
  • This study was designed to identify and quantitate airborne isocyanate simultaneously by HPLC. These samples were collected using 1-(2-pyridyl)piperazine(1-2PP) coated glass fiber filter from polyurethane painting works at 8 wood furniture factories in Kimpo and Inchun. The results obtained were as follows : 1. The most suitable mobile phase condition of simultaneously analyzing isocyanates was 0.01 M ammonium acetate buffer ACN(70/30) adjusted to pH 6.2 from the beginning of the analysis to 20 min and 0.01 M ammonium acetate buffer/ACN(50/50) adjusted to pH 6.2 from 21 min to 40 min using the gradient mode. The peaks of isocyanates were able to obtain within 30 min. 2. The recovery efficiencies for 2,6-TDI, 2,4-TDI, HDI and MDI urea derivates spiked at the target concentration on coated glass fiber tillers were 91.00, 93.42, 91.31 and 94.21 %, respectively. 3. The qualitative analysis of the isocyanates samples from polyurethane spray painting works in wood furnture factories identified Ihree isocyanates, 2,6-TDI, 2,4-TDI and MOI. And their concentration ranges were 0-312.6, 0-56.3 and $0-62.1{\mu}g/m^3$, respectively. A disadvantage of using the colorimetric method for isocyanate analysis is its inability of separating isocyanates. This study identified such three isocyanates as 2,6-TDI, 2,4-TDI and MDI from polyurethane spray painting works in wood furniture factories. These isocyanates were successfully quantitated by HPLC by modifying the mobile phase condition and switching to gradient mode.

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Thermostable Sites and Catalytic Characterization of Xylanase XYNB of Aspergillus niger SCTCC 400264

  • Li, Xin Ran;Xu, Hui;Xie, Jie;Yi, Qiao Fu;Li, Wei;Qiao, Dai Rong;Cao, Yi;Cao, Yu
    • Journal of Microbiology and Biotechnology
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    • v.24 no.4
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    • pp.483-488
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    • 2014
  • In order to improve the expression of heat-resistant xylanase XYNB from Aspergillus niger SCTCC 400264, XynB has been cloned into Pichia pastoris secretary vector pPIC9K. The XynB production of recombinant P. pastoris was four times that of E. coli, and the $V_{max}$ and specific activity of XynB reached $2,547.7{\mu}mol/mg$ and 4,757 U/mg, respectively. XynB still had 74% residual enzyme activity after 30 min of heat treatment at $80^{\circ}C$. From the van der Waals force analysis of XYNB (ACN89393 and AAS67299), there is one more oxygen radical in AAS67299 in their catalytic site, indicating that the local cavity is much more free, and it is more optimal for substrate binding, affinity reaction, and proton transfer, etc, and eventually increasing enzyme activity. The H-bonds analysis of XYNB indicated that there are two more H-bonds in the 33rd Ser of XYNB (AAS67299) than in the 33rd Ala(ACN89393 ), and two H-bonds between Ser70 and Asp67.

Determination of dextromethorphan and its metabolite dextrorphan in human urine by High-performance liquid chromatography

  • Son, Haeng-Ja;Park, Mee-Jung;Choi, Sang-Kil;Lim, Mi-Ae;Chung, Hee-Sun
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.279.2-280
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    • 2003
  • A simple and accurate reverse-phase high performance liquid chromatography (HPLC) coupled with photodiode array was developed for the determination of dextromethorphan(DM) and its metabolite dextrorphan(DX) in human urine. Chromatographic separation was accomplished on a cyano analytical column at 220 nm using a mobile phase containing 25 mM triethylammonium phosphate buffer(PH 3.0) in a 0-70% ACN gradient and triazolam(TZ) was used as internal standard(I.S). (omitted)

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Flail arm syndrome with several issues related to the diagnostic process

  • Kim, Jae-Youn;Park, Yun Kyung;Yoon, Bora;Lee, Kee Ook;Kim, Yong-Duk;Na, Sang-Jun
    • Annals of Clinical Neurophysiology
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    • v.19 no.1
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    • pp.68-70
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    • 2017
  • Flail arm syndrome (FAS), known as one of the atypical amyotrophic lateral sclerosis (ALS) variants, has a similar clinical course and pathologic findings as ALS. Therefore it is difficult to differentiate between ALS and FAS at a glance. There are few reports involving individual analysis of FAS patients to date. The findings of polysomnography (PSG) in patient with FAS are not well known. We report a male FAS patient with review of literatures and several issues related to the diagnostic process.