• 한국식품과학회지
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• 제48권5호
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• pp.405-412
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• 2016

성기능개선, 원기증강 등에 효과가 있는 것으로 판매되고 있는 식품 등에서 발기부전치료제 및 그 유사물질 등이 불법적으로 혼입되어 검출되고 있다. 이들 부정물질이 혼입된 불량식품은 안전성과 유효성이 입증되지 않았기 때문에 국민건강을 위협할 수 있다. 그러므로 본 연구에서는 식품과 가짜 발기부전치료제에 불법 혼입된 부정물질을 모니터링하기 위하여, 해외 인터넷 사이트와 오프라인 매장에서 성기능개선, 원기증진을 표방하는 식품과 최음제, 가짜 발기부전치료제 161건을 구입하였다. 시험방법의 유효성 검증을 위하여 선택성, 직선성, 검출한계, 정량한계, 정확성, 정밀성을 검토하였다. LC-PDA와 LC-MS/MS를 이용하여 부정물질 54종을 동시분석한 결과, 48건의 시료에서 7종의 부정물질(요힘빈, 이카린, 실데나필, 타다라필, 클로로프레타다라필, 데메틸실데나필, 디메틸치오실데나필)이 검출되었다. 성기능개선이나 최음제로 판매되는 제품에는 부정물질이 혼입될 가능성이 있으므로, 이들 제품을 구입할 때는 각별한 주의가 필요하다.

• 분석과학
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• 제21권2호
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• pp.65-83
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• 2008

식품에 첨가할 수 없는 의약품이나 화학합성물질이 함유된 부정유해식품이 증가하고 있는 실정이다. 특히 발기부전치료제 성분인 실데나필, 바데나필 및 타다라필의 화학구조를 변형한 미지의 물질이 검출되고 있다. 또한 기존 식품의 기준규격 검사에 따른 단속을 피하기 위하여 성기능강화 등 치료효능을 지닌 의약품 성분의 화학구조를 변형한 불법으로 합성한 부정유해물질은 안전성이 전혀 입증되지 않았으므로 그 위해성이 우려되고 있다. 따라서 식품의 안전성을 확보하기 위하여 발기부전치료제의 화학구조를 변형한 호모실데나필, 홍데나필, 슈도바데나필, 아미노타다라필, 하이드록시호모실데나필, 하이드록시홍데나필, 디메틸실데나필, 잔소안트라필, 하이드록시바데나필, 노르네오실데나필, 데메틸홍데나필, 피페리디노홍데나필, 카보데나필, 치오실데나필, 디메틸치오실데나필, 아세틸바데나필의 총 16개의 발기부전치료 성분의 유사물질 관련 자료와 식품 중 부정유해물질의 규명 및 분석 현황을 정리하였다.

• 한국식품과학회지
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• 제48권5호
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• pp.424-429
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• 2016

비만은 전세계적으로 심각한 문제로 인식되고 있다. 최근 체중감소와 유지를 위한 다이어트제품에 비만치료제와 그 유사물질, 사용금지 성분들이 발견되고 있다. 정부의 감시를 피하기 위하여, 비만치료제의 화학구조를 일부 변형시킨 유사물질이 지속적으로 합성되고 있다. 부정물질이 혼입된 다이어트식품을 신속하게 검사하기 위하여, 국내에서 판매되는 제품과 해외 인터넷 사이트에서 128건의 다이어트제품을 구매하였으며, HPLC-PDA와 LC-MS/MS로 21종의 부정물질을 동시분석하였다. 시험법의 유효성 검증은 선택성, 직선성, 검출한계, 정량한계, 정확성, 정밀성을 검토하였다. 분석결과 31건의 시료에서 부정물질이 검출되었으며, 검출수준은 시부트라민 9.9-135.3 mg/g, 요힘빈 0.2-17.5 mg/g, 이카린 1.8 mg/g이었다. 본 연구의 부정물질 분석법은 간단하면서도 신속한 분석법으로, 식품안전관리를 위한 기초자료로 활용될 수 있을 것으로 사료된다.

• 상하수도학회지
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• 제14권1호
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• pp.54-61
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• 2000

Recently, our circumstances are threatened by an accident that leakage of under ground storage tank and illegal dumping of synthetic organic compounds at chemical plants and many treatment methods, Activated carbon adsorption, Ozonization, Membrane filtration and Photocatalystic oxidation, are developed to remove such a synthetic organic compounds. And it has reported that Activated carbon adsorption have a great removal efficiency to nondegradable matters and organic compounds which have a high molecular weight. Comparing with other adsorbents, Activated carbon adsorption have a worse efficiency when ad desorption speed is low. Thus improved type of adsorbents was invented and one of those is Activated Carbon Filter. The purpose of this study was getting information about adsorption characteristic phenol which can be applied Activated Carbon Fiber and Granular Activated Carbon. In detail, With comparing removal characteristics of phenol in the presence Humic Acid using Activated Carbon Fiber(ACF) and Granular Activated. Carbon(GAC), it is to certify an effective application of Activated Carbon Fiber. At the range of this study, Batch test, Isotherm adsorption test and Factorial analysis, following conclusion were obtained from the results of this study. Batch test was carried to know time of adsorption equilibrium. In this study about time of adsorption equilibrium by ACF was faster than GAC's, for developed micropore of ACF. From the result of phenol adsorption test, High removal rate of adsorption is shown at pH 5. The result of lsotherm adsorption test, it has represented that the Freundlich's isotherm is most suitable one in others, that a ACF's adsorption capacity is more excellent than GAC's. Adsorption of phenol exiting humic acid is decreased getting raised humic acid concentration. Since ACF's micropore is developed at this time, an effect of high molecular humic acid is lower. Factorial analysis was carried to know about Main effect which was injection dosage of adsorbent in the range of this study.

• 분석과학
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• 제32권2호
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• pp.56-64
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• 2019

Recently, a number of adulterated products, which are advertised as hair-growth enhancer have been emerged among those who suffer hair loss disease. For continuous control of illegal products, in this study, a rapid and sensitive method for simultaneous screening of 12 compounds that enhance hair-growth was established to protect public health by ultrahigh-performance liquid chromatography coupled to quadrupole-orbitrap mass spectrometry (UHPLC-Q-Orbitrap-MS). Fragmentation pathways of them were proposed based on $MS^2$ spectral data obtained using the established method. In this analysis, the LODs and LOQs ranged from 0.05 to 50 ng/mL and from 0.17 to 167 ng/mL, respectively. The square of the linear correlation coefficient ($R^2$) was determined as more than 0.995. The intra- and inter-assay accuracies were respective 88-112 % and 88-115 %. Their precision values were measured within 5 % (intra-day) and 10 % (inter-day). Mean recoveries of target compounds in adulterated products ranged from 84 to 115%. The relative standard deviation of stability was less than 12 % at $4^{\circ}C$ for 48 h. The method was employed to screen 14 dietary supplements advertised to be effective for the treatment of hair loss. Some of the products (~21 %) were proven to contain synthetic drugs that promote hair growth such as triaminodil, minoxidil, and finasteride.

• 분석과학
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• 제20권1호
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• pp.78-83
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• 2007

식품 중 발기부전치료 성분 및 유사물질의 분석능력을 평가하기 위하여 실험실간 정도관리를 시도하였다. 평가대상물질은 실데나필, 타다라필, 바데나필, 호모실데나필, 하이드록시호모실데나필, 슈도바데나필 6종이었으며, 참여기관은 식품위생검사를 담당하고 있는 13개 기관이었다. 표준시료는 이중맹검을 위하여 평가대상물질 중 임의의 3종을 함유하도록 조제한 인삼음료 13개이었다. 분석방법은 식품공전의 일반시험법에 제시되어 있는 발기부전치료제 유사물질 시험법에 따라 일정량을 취하여 물에 희석한 후 유기용매로 추출하여 HPLC/UV로 분석하고 LC/MS로 확인하는 방법을 적용하였다. 분석기간은 표준시료를 수령한 날로부터 60일이었다. 검사능력관리규정에 따라 Z-값 및 RSZ를 종합평가한 결과 10기관이 만족한 수준이었다.

• 분석과학
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• 제29권4호
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• pp.155-161
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• 2016

Distribution of various illegal or counterfeit drugs of seven approved erectile dysfunction drugs and their analogues has been increased, causing health problems such as cardiovascular disorder, tachycardia, headache, or vision disturbance. We used liquid chromatography-electrospray ionization-tandem mass spectrometry (LC-ESI-MS/MS) to determine the erectile dysfunction drugs and their analogues in various counterfeit drugs. Eleven erectile dysfunction drugs and their analogues were detected, with sildenafil and its analogues being the most counterfeited compounds (73.8 %), followed by tadalafil and its analogues (25.4 %). The limits of detection (LOD) and the limits of quantitation (LOQ) of liquid-type and solid-type negative samples ranged from 0.1 to 3.3 ng/mL or ng/g and from 0.3 to 10.0 ng/mL or ng/g, respectively. The recoveries ranged from 84.3 to 112.3 % and 83.2 to 110.2 %, respectively. The contents of sildenafil and tadalafil in the various counterfeit drugs ranged from 21.0 to 947.5 mg/g and from 0.2 to 170.2 mg/g, respectively.

• 분석과학
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• 제31권4호
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• pp.171-178
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• 2018

Recently, for successful lactation, many breastfeeding mothers seek various products, including herbal medicine, dietary supplements, and prescribed medicines, to improve milk production. As demand for galactogogues grows, it is highly possible that pharmaceutical galactogogues may be adulterated with illegal products to maximize their efficacy. For continuous control and supervision of illegal products, we developed and validated a simple and sensitive LC-MS/MS method capable of simultaneously determining five galactogogues. Chromatographic separation was conducted using an Agilent Poroshell $120SB-C_{18}$ column with a mobile phase consisting of 20 mM ammonium formate (pH 5.4) and 100 % acetonitrile. The total run time was 13 min per analyte. The proposed method was performed according to the guidelines of the International Conference of Harmonization and it produced reliable results. This method showed high sensitivity and specificity, with a limit of detection (LOD) and limit of quantitation (LOQ) of 0.01-0.82 ng/mL and 0.02-2.45 ng/mL, respectively, for the solid- and liquid-type samples. Specificity was evaluated by analyzing matrix-blank samples spiked with the target compounds at LOQ levels, which provided a good separation of all peaks without interference. Additionally, the repeatability and intermediate precision were typically <15 %, whereas the recovery was 80-120 % of the values obtained using blank samples. Thus, we concluded that this method could be used for the identification and quantification of galactogogues in food or herbal products.

• Geomechanics and Engineering
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• 제18권4호
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• pp.427-437
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• 2019

Waste materials are being produced in huge quantities globally, and the usual practice is to dump them into legal or illegal landfills. Recycled tiles (RT) are being used in soil stabilisation which is considered as sustainable solution to reduce the amount of waste and solve the geotechnical problems. Although the stabilisation of soil using RT improved the soil properties, it could not achieve the standard values required for construction. Thus, this study uses 20% RT together with low cement content (2%) to stabilise soft soil. Series of consolidated undrained triaxial compression tests were conducted on untreated and RT-cement treated samples. Each test was performed at 7, 14, and 28 days curing period and 50, 100, and 200 kPa confining pressures. The results revealed an improvement in the undrained shear strength parameters (cohesion and internal frication angle) of treated specimens compared to the untreated ones. The cohesion and friction angle of the treated samples were increased with the increase in curing time and confining pressure. The peak deviator stress of treated samples increases with the increment of either the effective confining pressures or the curing period. Microstructural and chemical tests were performed on both untreated and RT-cement treated samples, which included field emission scanning electron microscopic (FESEM), Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD), and energy dispersive X-ray spectrometer (EDX). The results indicated the formation of cementation compounds such as calcium aluminium hydrate (C-A-H) within the treated samples. Consequently, the newly formed compounds were responsible for the improvement observed in the results of the triaxial tests. This research promotes the utilisation of RT to reduce the amount of cement used in soil stabilisation for cleaner planet and sustainable environment.

• 분석과학
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• 제26권4호
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• pp.228-234
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• 2013

국내에서 불법 유통 되거나 남용되고 있는 methamphetamine은 아민을 함유한 불법약물로서 그에 대한 신속하고 용이한 동정 및 정량적인 분석 방법은 불법약물 검사의 중요한 이슈가 되어왔다. 새로운 screening방법을 모색하기 위해 methamphetamine과 구조적으로 유사한 3종의 유기 화합물을 silica gel ($SiO_2$) TLC상에서 N-(9-Fluorenylmethoxycarbonyloxy)succinimide (FMOC-NHS)와 반응을 시켰다. TLC상 반응 생성물을 일반 유기합성 경로로 합성한 대조물질과 비교 확인한 다음, 이 방법의 검출한계(Limit of detection)를 조사하였다. 실험결과 유도체화 시약으로 사용한 FMOC-NHS는 TLC상에서 1차 및 2차 아민과 반응하여 UV-active한 화합물을 생성시키는 것을 확인하였다. 2D TLC 실험에서는 0.045-0.01 mg/mL ($2{\mu}L$ per spot), 그리고 1D co-spot TLC 실험에서 0.002-0.007 mg/mL ($2{\mu}L$ per spot)의 검출한계는 유도체화 시약의 농도에 대한 의존성을 나타내었다.