• 대한수의학회지
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• 제41권1호
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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.

• 대한화학회지
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• 제43권4호
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• pp.438-446
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• 1999

오존처리의 소독 부산물인 알데하이드류를 HPLC로 분석하는 최적 분석법을 확립하였다. 예비실험을 통하여 알데하이드류는 포름알데하이드, 아세트알데하이드, 아크롤레인, 프로피온알데하이드, 부틸알데하이드, 벤즈알데하이드 6종과 케톤류인 아세톤 1종 모두 7종을 대상 시료로 선정하였다. HPLC에 의한 알데하이드-DNPH 유도체를 최적화 하기 위해 시트르산 완충용액의 pH, 반응 온도, 반응 시간, DNPH 농도, 추출 용매의 종류 및 조성의 최적 조건을 구하였다. 그 결과 시트르산 완충 용액의 pH는 3.0, 반응 온도는 40$^{\circ}C$, 반응시간은 15분, DNPH의 농도는 0.012%에서 최적 반응 조건임을 알 수 있었으며, 반응이 완결된 알데하이드-DNPH 유도체를 $C_18$Sep-Pak 카트리지에 농축시켜 과량의 DNPH를 용리시킨 다음 탈착용매로서 THF/ACN=70/30의 혼합용매 2mL로 탈착하였을 때 87∼107% 범위의 회수율을 나타내었다. HPLC 분리 조건으로서 Nova-Pak $C_18$ 컬럼상에서 이동상의 초기 조건은 ACN/MeOH/Water=30/10/60 에서 최종 조건은 80% ACN으로 하는 기울기 용리를 수행하였을 때 7종의 알데하이드류가 20분 이내에 용리되면서 모두 거의 기준선 분리가 되었다. 본 실험에서 확립한 알데하이드-DNPH 유도체의 최적 분석 조건과 EPA Method 554와 회수율을 비교한 결과, 본 실험에서는 86∼103%, EPA Method 554로부터는 84∼103%으로 거의 일치한 결과를 나타내었다.

• Korean Chemical Engineering Research
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• 제49권6호
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• pp.829-834
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• 2011

난백에 함유된 lysozyme은 용균작용을 하며 ovalbumin은 면역계에서 항원으로써 역할을 한다. 난백분석에는 일반적으로 전기영동, 겔 투과 크로마토그래피, reversed-phase HPLC(RP-HPLC)를 사용하는데 신속한 분석을 위해 RPHPLC가 사용된다. HPLC 컬럼으로 C18 컬럼(Agilent, USA)을 사용하였다. 최적의 분리조건을 찾기 위해 이동상의 조성과 온도를 변화하였고 용량인자, 분리도를 계산하여 그 값을 비교하였다. 등용매 용리에서 acetonitrile(ACN), distilled ater(DW), trifluoroacetic acid(TFA)의 이동상 부피비를 30/70/0.1~60/40/0.1로 ACN 부피비를 10%씩 증가시키며 실험하였고 이 때 온도는 $20^{\circ}C$이었다. 기울기 용리에서는 ACN과 증류수의 비율을 20분 동안 10/90~60/40으로 증가시켰고 20, 30, $40^{\circ}C$의 온도변화를 주었다. 등용매 용리에서 이동상 조성이 50/50/0.1일 때 세 개의 피크로 분리되었고 개의 피크 중 첫 번째 피크가 lysozyme, 세 번째 피크가 ovalbumin임을 확인하였다. 기울기 용리에서는 온도가 $30^{\circ}C$일 때 네 개의 피크가 나왔으며 네 개의 피크 중 첫 번째 피크가 lysozyme, 세 번째 피크가 ovalbumin임을 확인하였다.

• Mass Spectrometry Letters
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• 제9권2호
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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.

• 한국환경보건학회지
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• 제22권2호
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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.

• 한국식품과학회지
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• 제30권6호
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• pp.1252-1258
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• 1998

재배 면적이 비교적 넓은 국내산벼 10품종 백미의 알콜용해성단백질을 capillary elictrophoresis로 분석하고 품종간 단백질 pattern의 차이를 비교 분석하므로써 신속한 품종판별법으로서의 적용가능성을 검토하였다. P-ACN buffer를 이용한 분석조건에서 각 품종은 25분 이내에 분석완료 되었으며 peak pattern의 특징에 따라 동진벼 group, 추청벼 group 및 일품벼 group의 3group으로 분류할 수 있었다. 동진벼, 계화벼, 영남벼가 동진벼 group으로 분류되었으며 이 group에서는 다른 품종에서는 거의 나타나지 않은 peak h가 전체 peak area의 $6{\sim}8%$를 차지하며 뚜렷이 검출되었다. 추청벼 group은 peak h를 제외한 대부분의 peak가 동진벼 group과 비슷하게 나타났으며 추청벼, 오대벼, 만금벼 및 봉광벼 4품종이 해당되었다. 일품벼 group으로 분류된 일품벼, 화성벼 및 화영벼에서는 peak g가 전체 peak의 약 70%라는 압도적인 비율을 나타내었다. 주요 peak의 뚜렷한 차이에 따라 3 group으로 분류하기는 하였으나 일품벼, 오대벼 등의 일부 품종은 단독으로 구별이 가능하였으며 각 group 내에서도 미미하기는하나 구성 peak들을 면밀히 비교 분석하므로써 품종에 따른 특성을 도출할 수 있었다. 또한 다른 분석법과 비교할 때 우리 나라에서 재배면적이 50% 이상으로 가장 많은 동진벼와 추청벼는 각 현미의 윗면, 측면, 앞면의 화상을 이용한 품종판별법에서 서로 오판될 확률이 비교적 높았으나 CE로는 peak h에 의해 서로 쉽게 구분되었다.

• 한국산업보건학회지
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• 제4권2호
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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.

• Journal of Microbiology and Biotechnology
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• 제24권4호
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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.

• 대한약학회:학술대회논문집
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• 대한약학회 2003년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.1
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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)

• Annals of Clinical Neurophysiology
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• 제19권1호
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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.