• 한국동물위생학회지
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• 제30권1호
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• pp.1-12
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• 2007

A liquid chromatographic method has been developed for the analysis of aminoglycoside antibiotics (AMGs) using Heptafluorobutyric acid (HFBA) as a ion-pairing reagent. AMGs (amikacin, apramycin, dihydrostreptomycin, gentamicin, hygrosin B, kanamycin, neomycin, spectinomycin and tobramycin) were formed by reaction with HFBA as ion-pairing reagent. HFBA was attached to corresponding amino group of AMGs. These AMGs compounds were separated and detected by electrospray ionization mass spectrometry (ESI-MS). The experimental conditions for separation of AMGs were optimized and validated. A simple liquid chromatographic method for the determination of AMGs was demonstrated.

• 분석과학
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• 제21권6호
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• pp.543-552
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• 2008

식품 중 클로로프로판올 화합물인 3-MCPD (3-monochloropropane-1,2-diol, $C_3H_7ClO_2$, MW. 110) 및 1,3-DCP (1,3-dichloropropan-2-ol, $C_3H_6Cl_2O$, MW. 128)를 분석하는 효과적인 방법을 확립하였다. 시료를 5M NaCl용액으로 균질화 한 후 알루미늄옥사이드와 섞어 유리컬럼에 충진하고 디클로로메탄으로 시료 중 클로로프로판올 화합물을 용출하였다. 용출된 클로로프로판올 화합물은 감압증류장치와 질소가스로 농축한 뒤 HFBA (Heptafluorobutyric anhydride, $C_8F_{14}O_3$, MW. 410)로 유도체화하여 GC/MS로 분석하였다. 3-MCPD-HFBA 유도체화 화합물(MW. 502)은 m/z 253, 275, 289, 291, 453를 선택이온으로 하고 1,3-DCP-HFBA 유도체화 화합물(MW. 325)은 110, 275, 277를 선택이온으로 설정하여 정성 정량 하였다. 확립된 분석법의 정량한계는 3-MCPD 및 1,3-DCP 모두 0.01 mg/kg이었고, 0.01~1.00 mg/kg의 농도범위에서 직선성($R^2{\geq}0.999$)이 좋았으며 평균회수율은 약 97%내외였다. 확립된 분석법을 이용하여 다양한 식품 중 클로로프로판올 화합물을 조사한 결과, 0.0~0.3 mg/kg (n=56/157) 수준으로 3-MCPD로 검출되었다.

• 분석과학
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• 제17권4호
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• pp.322-336
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• 2004

항암치료제인 tamoxifen을 복용한 후 체내에서 분비되는 tamoxifen과 그 대사체를 trifluoroacetic anhydride (TFAA), pentafluoropropionic anhydride (PFPA), 및 heptafluorobutyric anhydride (HFBA) 유도체화 시약으로 이들이 함유하고 있는 히드록시기를 아실화반응시킴으로써 기체크로마토그래피와 질량분석기로 분석 가능하게 하고, 검출한계 등을 개선한 새로운 방법에 대해 연구하였다. 한편 질량 분석기로 검출하기 위한 이온화 방법의 하나인 전자 충격 이온화법과 화학 이온화법을 비교하여 보다 개선된 분석법을 연구하고, 이 방법을 실제 인체 뇨시료에 적용한 tamoxifen 대사체 검출을 위한 최적 조건을 연구하였다. Acylation 방법에 있어서의 최적 반응조건은 반응 온도 $50^{\circ}C$와 반응 시간 30 min 이었으며, 뇨시료에 있어서 tamoxifen 대사체 추출에 대한 최적 pH는 7.0, 추출 용매는 디에틸에테르가 적절함을 알 수 있었다. TFAA, PFPA, HFBA로 유도체 시킨 후 CI법과 EI법을 비교 분석한 결과, NCI법에서는 주로 $[M-HF]^-$ 또는 $[M-2HF]^-$이온이 주요 이온으로 나타났으며 NCI에서 감도가 뛰어난 할로겐원소가 함유된 유도체 시약을 사용하였기 때문에 생체시료 내에 미량 존재하는 약물을 보다 용이하게 검출 및 확인 할 수 있었다. 한편 GC/MS로 tamoxifen대사체를 분석한 결과 tamoxifen이 간에서 대사 될 때 주 대사체로 알려져 있는 4-hydroxytamoxifen은 검출 되지 않았고 hydroxymethoxytamoxifen이 주 대사체로 검출되었다. Acylation 유도체화 과정을 거친 hydroxymethoxytamoxifen은 NCI에서의 토막 이온을 조사한 결과 아미노 그룹의 ${\beta}$-cleavage가 일어난 m/z 491이온, acylation 유도체 한 분자가 쪼개진 m/z 344이온이 비교적 높게 검출되었다.

• Journal of Photoscience
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• 제9권1호
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• pp.23-28
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• 2002

In order to obtain thermal-stable, low birefringent, and low optical loss waveguiding materials, we synthesized several fluorinated poly (maleimide-co-glycidylmethacrylate)s using a pentafluorophenylmaleimide (PEM) and two kinds of methacrylate derivatives as comonomers and glycidylmethacrylate as a crosslinker. One comonomer is a linear fluorinated methacrylate (HFBM) and another is a bulky norbornane-derived methacrylate (NMMA). These copolymers could be self-crosslinked by heating due to epoxy groups of glycidylmethacrylates. As a maleimide contents increased to 50 mol%, these copolymers showed high decomposition temperatures of above 300$^{\circ}C$. The refractive index could be precisely controlled by the variation of PFM/HFBA or PFM/NMMA feed ratio in the range of 1.410∼1.508 at 643 nm. The copolymers had very low birefringence in the range of 1∼5${\times}$10$\^$-4/.

• Bulletin of the Korean Chemical Society
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• 제33권2호
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• pp.559-563
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• 2012

An analytical method for the simultaneous determination of veterinary medicines (amprolium and decoquinate) in cattle and chicken's muscle by HPLC/UV-vis was established. Samples were extracted by a HLB (Hydrophilic-Liphophilic Balance) cartridge with acetonitrile and methanol. Prior to HPLC injection, a mixture solvent (Water:MeOH, 1:1) was utilized as a reconstitution solvent. Chromatographic separation was achieved with a C18 column ($250{\times}4.6mm$, $5{\mu}m$) using gradient elution with 20 mM HFBA and MeOH:ACN (1:1.8). The calibration curves from the spiked blank matrix showed good linearity (above $r^2$=0.997) in the concentration range of $0.13-12.0mg\;kg^{-1}$. The relative recovery (accuracy) and limit of quantitation (LOQ) were in the range of 78.5-107.1% and $0.13-0.42mg\;kg^{-1}$, respectively. The developed method can be used to determine under the MRL (Maximum Residue Limits) levels of veterinary medicines in animal tissues.

• 한국산업보건학회지
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• 제7권1호
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• pp.49-59
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• 1997

This study was performed to analyze the purity of technical grade ${\alpha}$-naphthylamine, to establish optimal analytical condition of ${\alpha}$-naphthylamine in urine and to determine the urine sample of workers exposed to ${\alpha}$-naphthylamine. The purity of technical grade ${\alpha}$-naphthylamine were $96.5{\pm}2.38%$, $94.1{\pm}0.97%$, $97.0{\pm}0.02%$ by gas chromatography-mass selective detector. To analyze ${\alpha}$-naphthylamine in urine, high performance liquid chromatography-electrochemical detector and gas chromatography-electron capture detector operating conditions have been optimized by preliminary expriment. In high performance liquid chromatography-electrochemical detector, the mobile phase was consisted of acetonitrile(35%) and water(65%), and the flow rate was maintained at 1.0ml per minute. Optimal detective condition was 9.0V(10nA/V) of electrochemical detector. The recovery of sep-pak treatment method was highly estimated as pretreatment of ${\alpha}$-naphthylamine in urine. The free amine was isolated by gas chromatography-electron capture detector after basic hydrosis, sep-pak treatment, toluene elution and HFBA(heptafluoro-butyric anhydride) derivatization of urine. The recovery of ${\alpha}$-naphthylamine in urine was $98.73{\pm}3.29%$ by gas chromatography-electron capture detector. The sensitivity was more higher than that of high performance liquid chromatography-electrochemical detector. Urinary ${\alpha}$-naphthylamine was detected in only one worker among nine workers. The level of ${\alpha}$-naphthylamine in urine was 6.42 ng/ml.

• Bulletin of the Korean Chemical Society
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• 제30권7호
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• pp.1497-1504
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• 2009

GC/MS analysis of catecholamines (CAs) in biological sample may produce poor reproducible quantitaion when chemical derivatization is used as the technique to form a volatile derivative. Significant quantities of the side products can be formed from CAs with primary amine during the derivatization reaction under un-optimized conditions. We have tested various chemical derivatization techniques in an attempt to find an optimum derivatization method that will reduce side product formation, enable to separate several catecholamine derivatives in GC chromatogram, and obtain significant improvement of detection sensitivity in GC/MS analysis. Whereas several derivatization techniques such as trimethylsilylation (TMS), trifluoroacylation (TFA), and two step derivatization methods were active, selective derivatization to form O-TMS, N-heptafluorobutylacyl (HFBA) derivative using N-methyl-N-(trimethylsilyl)-trifluoroacetamide (MSTFA) and N-methyl-bis(heptafluorobutyramide) (MBHFBA) reagents was found to be the most effective method. Moreover, this derivative formed by selective derivatization could provide sufficient sensitivity and peak separation as well as produce higher mass ion as base peak to use selected ion in SIM mode. Calibration curves based on the use of an isotopically labeled internal standard show good linearity over the range assayed, 1 ~ 5000 ng/mL, with correlation coefficients of > 0.996. The detection limits of the method ranged from 0.2 to 5.0 ppb for the different CAs studied. The developed method will be applied to the analysis of various CAs in biological sample, combined with appropriate sample pretreatment.

• 분석과학
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• 제22권3호
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• pp.210-218
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• 2009

GC-MS/MS를 이용하여 모발 중 암페타민계 마약류 4종과 노르케타민의 동시 분석법을 확립하였으며 결과의 신뢰도를 높이기 위해 분석법 검정을 실시하였다. 모발 시료의 전처리 과정은 증류수와 아세톤을 이용하여 세척, 자동분쇄기를 이용한 세절, 메탄올 용매를 이용한 추출 및 배양 그리고 HFBA로 유도체화하는 단계를 거쳐 GC-MS/MS를 이용하여 분석하였다. 그 결과 모든 분석물질에 대해 정량범위 내에서 우수한 직선성을 나타내었으며, 실제 마약 복용자의 모발감정에 이용될 수 있는 충분한 감도와 선택성, 정밀도와 정확도를 확인하였다. 검정곡선의 결정계수($r^2$)는 0.998 이상을 나타내었고 검출 한계는 0.007 ng/mg 이하였으며 회수율은 75.9-100.9%이었다. 일내 (intra-day) 및 일간 (inter-day) 정확도는 -2.6-17.0%의 범위를 나타내었으며 정밀도는 10.7%이하로 모두 기준값(20% 이하)이내의 값을 나타내었다. 확립된 분석법을 마약 복용자의 모발에 적용한 결과 메스암페타민의 농도 분포는 0.97-19.30 ng/mg이었으며 암페타민은 0.14-2.56 ng/mg이었다.