• Environmental Engineering Research
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• 제20권2호
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• pp.127-132
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• 2015

Perfluorooctane sulfonate (PFOS) and Perfluorooctanoic acid (PFOA) are persistent environmental pollutants, extremely stable, and possibly adversely affect human health. They are widely used in many industries and consumer goods, including sunscreen products. These substances are stable chemicals made of long carbon chains, having both lipid- and water-repellent qualities. The research objectives are (1) to find the most effective method for the preparation of semi-liquid samples by comparing solid phase extraction (SPE) and centrifugation after Pressurized liquid extraction (PLE), and (2) to determine the contamination levels of PFOS and PFOA in waterproof sunscreen samples. All sunscreen samples were analyzed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). Sunscreen samples were purchased from domestic and international brands sold in Thailand. Special chemical properties were considered for the selection of samples, e.g., those found in waterproof, sweat resistant, water resistant, and non-stick products. Considering the factors of physical properties, e.g., operation time, chemical consumption, and recovery percentage for selecting methods to develop, the centrifugation method using 2 mL of extracted sample with the conditions of 12,000 rpm and $5^{\circ}C$ for 1 hour after PLE was chosen. The highest concentrations of PFOS and PFOA were detected at 0.0671 ng/g and 21.0644 ng/g, respectively. Even though present concentrations are found at ng/g levels, the daily use of sunscreen products is normally several grams. Therefore, a risk assessment of PFOS and PFOA contamination in sunscreen products is an important concern, and more attention needs to be paid to the long-term effects on human health.

• 한국대기환경학회지
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• 제34권1호
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• pp.120-143
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• 2018

The analytical methods and their ambient levels of organic nitrogenous compounds such as nitrosamines, nitramines (nitroamines), imines, amides and nitro-polycyclic aromatic hydrocarbons (nitro-PAHs) in the atmosphere are summarized and discussed. Sampling for the analysis of organic nitrogenous compounds was mostly conducted using high volume air sampler. The direct liquid extraction (DLE) using sonification and the pressurized liquid extraction (PLE) using the accelerated solvent extraction (ASE) have been frequently employed for the extraction of organic nitrogenous compounds in the atmospheric samples. After extraction, clean-up via filtration and the solid phase extraction (SPE) and concentrations using nitrogen and rotary evaporator have been generally conducted but in some studies the clean-up and concentration steps have been omitted to prevent the loss of analyte and improve the recovery rate of the analytical procedure. Instrumental analysis was mainly carried out using gas chromatography (GC) or the high performance liquid chromatography (HPLC) coupled with the single quadrupole mass spectrometer or tandem mass spectrometer in the electron ionization (EI), positive chemical ionization (PCI) and negative chemical ionization (NCI) mode and analysis sensitivity of nitrosamines and nitramines were higher in NCI mode. Desirable sampling and analysis methods for analyzing particulate organic nitrogenous compounds are suggested.

• 한국방사성폐기물학회:학술대회논문집
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• 한국방사성폐기물학회 2017년도 추계학술논문요약집
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• pp.223-224
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• 2017

• 상하수도학회지
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• 제32권6호
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• pp.559-572
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• 2018

The aim of this study was to evaluate pretreatment methods for 27 pharmaceuticals and personal care products (PPCPs) in various sewage samples using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) and online solid-phase extraction with LC-MS/MS. Extraction efficiencies of PPCPs in the solid phase under different experimental conditions were evaluated, showing that the highest recoveries were obtained with the addition of sodium sulfate and ethylenediaminetetraacetic acid disodium salt dehydrate in acidified conditions. The recoveries of target compounds ranged from 91 to 117.2% for liquid samples and from 61.3 to 137.2% for solid samples, with a good precision. The methods under development were applied to sewage samples collected in two sewage treatment plants (STPs) to determine PPCPs in liquid and solid phases. Out of 27 PPCPs, more than 19 compounds were detected in liquid samples (i.e., influent and effluent) of two STPs, with concentration ranges of LOQ-33,152 ng/L in influents and LOQ-4,523 ng/L in effluents, respectively. In addition, some PPCPs such as acetylsalicylic acid, ibuprofen, and ofloxacin were detected at high concentrations in activated sludge as well as in excess sludge. This methodology was successfully applied to sewage samples for the determination of the target compounds in STPs.

• 분석과학
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• 제19권5호
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• pp.441-448
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• 2006

소변 중 대마 남용여부를 판별하는데 기준이 되는 tetrahydrocannabinol (THC)의 대사체 성분인 11-nor-9-carboxy-${\Delta}^9$-tetrahydrocannabinol (THCCOOH)를 고체상 추출법 (solid-phase extraction, SPE)과 가스크로마토그래피/질량분석법 (GC/MS)을 이용하여 신속하게 분석 할 수 있는 방법을 제시하였다. 본 실험은 시험관에 소변 3 mL를 취해 염기성 (pH 10) 조건에서 가수분해 한 후, 양이온교환 카트리지를 사용하여 THCCOOH 성분을 선택적으로 추출하고, 증발 건고한 다음 유도체 반응을 시켜 GC/MS로 분석하였다. 그 결과 분석방법의 검출한계 (LOD)는 0.4 ng/mL이고, 정량한계 (LOQ)는 1.2 ng/mL이였다. 검정곡선의 직선성 상관계수 ($r^2$)는 1.2 (LLE는 1.3)~50.0 ng/mL의 농도범위에서 0.999를 나타내었다. 그리고 정밀도 (precision)와 정확도 (accuracy)는 모두 ${\pm}1.20%$ 이내로 안정적이었으며, 회수율(recovery)은 83.6~90.7%로 측정되었다. 액체상 추출법 (liquid-liquid extraction, LLE)과 비교할 때, SPE 방법이 회수율은 낮았지만 검출한계, 정량한계, 정밀도 및 정확도에서는 큰 차이가 없었다. 그러나 LLE 방법은 추출과정에 시간과 노력이 많이 드는 반면, SPE 방법은 상대적으로 추출 조작이 간편하고 신속하게 추출되었으며, 추출 잔류물도 깨끗하였다. SPE를 이용한 추출방법을 다수의 대마 흡연자 소변에 적용하였을 때 기존에 사용하던 LLE 방법보다 간편하고, 신속하게 대마 대사체 분석이 가능하였다.

• Food Science and Biotechnology
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• 제18권2호
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• pp.565-569
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• 2009

This study was conducted to evaluate the effects of different preparation methods on the recovery and quantification of ginsenosides in raw Korean ginseng (Panax ginseng C.A. Meyer). Eight major ginsenosides ($Rb_1$, $Rb_2$, $Rb_3$, Rc, Rd, Re, Rf, and $Rg_1$) were analyzed by high performance liquid chromatography (HPLC), after which the recovery and repeatability of the extraction of those ginsenosides using 3 different preparation methods were compared [A. direct extraction (DE) method, hot MeOH extraction/evaporation/direct dissolution; B. solid phase extraction (SPE) method, hot MeOH extraction/evaporation/dissolution/$C_{18}$ cartridge adsorption/MeOH elution; C. liquid-liquid extraction (LLE) method, hot MeOH extraction/evaporation/dissolution/n-BuOH fractionation]. Use of the DE method resulted in a significantly higher recovery of total ginsenosides than other methods and a relatively clear peak resolution. Use of the SPE and LLE methods resulted in clearer peak resolution, but lower ginsenoside recovery than the DE method. The LLE method showed the lowest ginsenoside recovery and repeatability among the 3 methods. Given that the DE method employed only extraction, evaporation, and a dissolution step (avoiding complicate and time consuming purification), this technique may be an effective method for the preparation and quantification of ginsenosides from raw Korean ginseng.

• Mass Spectrometry Letters
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• 제8권4호
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• pp.90-97
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• 2017

Androgenic anabolic steroids (AASs) are synthetic derivatives of testosterone with a common structure containing cyclopentanoperhydrophenanthrene nucleus. Their use enhances the muscle building capacity and is beneficial during performance. The AASs are one of the most abused group of substances in horse doping. Liquid chromatography tandem mass spectrometry ($LC/MS^n$) has been successfully applied to the detection of anabolic steroids in biological samples. However, the saturated hydroxysteroids viz: nandrolone, $5{\alpha}-estrane-3{\beta}$, $17{\alpha}-diol$ exhibit lower detection responses in electrospray ionisation (ESI) because of their poor ionisation efficiency. To overcome this limitation pre-column chemical derivatization has been introduced to enhance their detection responses in $LC-ESI-MS^n$ analysis. The aim of present study was to develop a sensitive method for identification and confirmation of nandrolone and its metabolite in horse urine incorporating pre-column derivatization using picolinic acid. The method consists of extraction of targeted steroid conjugates by solid phase extraction (SPE). The eluted steroid conjugates were hydrolysed by methanolysis and free steroids were recovered with liquid-liquid extraction. The resulting steroids were derivatized to form picolinoyl esters and identification was done using LC-ESI-MS/MS in positive ionization mode. The picolinated steroid adduct enhanced the detection levels in comparison to underivatized steroids.

• Asian-Australasian Journal of Animal Sciences
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• 제14권10호
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• pp.1465-1469
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• 2001

A sensitive high-performance liquid chromatographic method was developed to determine the content of cholesterol in milk and dairy products. To optimize separation of cholesterol, mobile phases including acetonitrile:2-propanol (8:1, v/v), acetonitrile:methanol (3:1, v/v), and acetonitrile:methanoI:2-propanol (7:3: I, v/v/v) were compared. Acetonitrile/methanol/2-propanol was superior to the other mobile phase systems for separating cholesterol. Liquid-liquid extraction (LLE) of cholesterol was simplified using a non-polar solvent, hexane, to remove interfering compounds, and had an excellent recovery $(100{\pm}1.0%)$ of cholesterol. A solid phase extraction (SPE) method using Sep-pak $C_{18}$ was developed and compared with LLE. The SPE method was rapid and highly reproducible. Both extraction methods were useful when used in combination with saponification of esterified cholesterol to facilitate total cholesterol determination. The detection limit of cholesterol was $0.01{\mu}g$. The newly developed HPLC method was rapid, simple, and accurate, and has advantages over the many methods commonly used.

• The Korean Journal of Physiology and Pharmacology
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• 제2권6호
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• pp.779-786
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• 1998

A reversed-phase high-performance liquid chromatogrphy (RP-HPLC) has been developed to analyze the metabolites of arachidonic acid based on the specificities of ultraviolet absorption of these various metabolites and is sensitive to the nanogram level. This procedure makes it possible to extract complex mixtures of eicosanoids efficiently with a single step and to analyze them simultaneously by RP-HPLC from biological samples using octadesylsilyl silica extraction column and $PGB_2$ as an internal standard. The cyclooxygenase products {prostaglandin $(PG)D_2,\;PGE_1,\;PGE_2,\;PGF_{1{\alpha}},\;PGF{2{\alpha}},\;6-keto-PGF_{1{\alpha}},$ and thromboxane $B_2(TXB_2)}$ and lipid peroxidation product, isoprostanes, of arachidonic acid were monitored by one isocratic HPLC system at 195 nm wavelength. The lipoxygenase products ${leukotriene(LT)B_4,\;LTC_4,\;LTD_4,$ and 5-hydroxyeicosatetraenoic acid (5-HETE), 12-HETE, 15-HETE} were measured by another isocratic HPLC system at 280 nm for LTs and 235 nm for HETEs. This method provides a simple and reliable way to extract and assess quantitatively the final arachidonic acid metabolites.

• 대한화학회지
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• 제31권3호
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• pp.244-249
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• 1987

미생물의 대사산물 중에서 각각의 균주에 특징있게 생성되는 탄소수 $C_2-C_5$인 휘발성 유리산의 정성 정량 분석자료는 혐기성 미생물을 확인하는 정보를 준다. 수용성 매체에 용해되어 있는 미생물의 대사산물을 처리함에 있어서 흡착제로 Chromosorbp를 사용한 liquid-solid extraction 방법에 대하여 조사 검토하였다. Chromosorb P는 친수성인 흡착제이므로 그 표면에 간섭물질인 수용성 성분들이 흡착되어 남아있는 반면에 비이온화성인 휘발성 유리산들은 ether에 의해서 정량적으로 회수가 된다. 이와 같이 신속하며 효율적으로 처리된 시료를 5% Carbowax 20M/0.75% $H_3PO_4$로 coating 된 stainless steel capillary column 으로 정성 정량분석하였다.