• Mass Spectrometry Letters
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• 제5권1호
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• pp.30-33
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• 2014

A solid phase extraction (SPE) method was optimized for the quantitative analysis of perfluorooctanoic acid (PFOA) in serum using hydrophilic-lipophilic balance SPE and LC-MS/MS. Fetal bovine serums spiked with $^{13}C_8$-PFOA before or after SPE were used as test samples for evaluation of the SPE efficiency. Simultaneous evaluation of matrix effects and absolute SPE recovery for $^{13}C_8$-PFOA in serum using different sample pre-treatments and SPE conditions allowed optimization of SPE process efficiency with minimal matrix effect and decent SPE recovery. Introduction of protein precipitation as a sample pre-treatment procedure for serum samples before SPE generally decreased matrix effect in LC-MS/MS analysis and provided more stable recovery of PFOA.

• Mass Spectrometry Letters
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• 제2권1호
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• pp.12-15
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• 2011

The Korean government has regulated emission of polychlorinated dibenzo-p-dioxins and dibenzofurans (PCDD/Fs) in waste water of manufacturing facilities producing chlorinated compounds since 2009. As this regulation is expected to be reinforced in 2013 to 50 pg I-TEQ/L, a large sample volume is required for the analysis of trace amounts of PCDD/Fs in waste water. Liquid-liquid extraction (LLE) is used to extract PCDD/Fs from aqueous samples; however, its low efficiency makes it inadequate for analyzing large sample volumes. Herein, we present a disk-type solid-phase extraction (SPE) method for the analysis of dioxin at a part per quadrillion level in waste water. This SPE system contains airtight glass covers with a decompression pump, which enables continuous semi-automated extraction. Small (0.5 L) and large (7 L) samples were extracted using LLE and SPE methods, respectively. The method detection limits (MDLs) were 0.001.0.25 and 0.015.4.1 pg I-TEQ/L for the SPE and LLE methods, respectively. The concentrations of detected congeners with both methods were similar. However, the concentrations of several congeners that were not detected with the LLE method were quantified using the SPE method.

• Bulletin of the Korean Chemical Society
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• 제30권1호
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• pp.61-66
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• 2009

An analytical method based on solid-phase extraction and gas chromatography / mass spectrometry has been developed for measurement of acaricides (amitraz, bromopropylate, coumaphos, cymiazole, and tetradifon) in honey sample. In the stability test of acaricides in honey, amitraz underwent a rapid degradation into 2,4-dimethylaniline (DMA), 2,4-dimethylphenylformamide (DMPF), and N-(2,4-dimethylphenyl)-N'-methylformamidine (DMPMF), whileas other acaricides were found to be stable even for over three months. Extraction of five acaricides from 5g of honey sample was carried out by liquid-liquid extraction using 20mL of ethylacetate. For purification, Florisil-SPE cartridge with elution of 5mL of n-hexane/ acetone (55:45, v/v) was found to remove interferences effectively. Quantification was performed using gas chromatography / mass spectrometry in the selected ion monitoring mode. Spiking experiments were carried out to determine the recovery, precision, and limits of detection (LODs) of the method. The overall recovery values from honey spiked at 0.02 and 0.20 ${\mu}g/g$ levels, respectively, were found to be greater than 75% for all acaricides. The method detection limits for acaricides were ranged from 0.1 to 3 ppb. The developed method in this study was applied for the monitoring of acaricides in honey products collected from urban markets in Korea.

• 식품보건융합연구
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• 제10권3호
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• pp.19-22
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• 2024

The field of synthetic biology has emerged in response to the ongoing progress in the life sciences. Advances have been made in medicine, farming, eating, making materials, and more. Synthetic biology is the exploration of using living organisms to create new organisms. By manipulating specific genes to express targeted proteins, proteins can be created that are both productive and cost-effective. Solid-phase extraction (SPE) and liquid-liquid extraction (LLE) are employed for protein separation during the production process involving microorganisms. This study centers on Scanning Probe Microscopy (SPM) to showcase its utility in the food industry and food management. SPE is predominantly utilized as a pretreatment method to eliminate impurities from samples. In comparison to LLE, this method presents benefits such as decreased time and labor requirements, streamlined solvent extraction, automation capabilities, and compatibility with various other analytical instruments. Anion exchange chromatography (AEC) utilizes a similar methodology. Pharmaceutical companies utilize these technologies to improve the purity of biopharmaceuticals, thereby guaranteeing their quality. Used in the food and beverage industry to test chemical properties of raw materials and finished products. This exemplifies the potential of these technologies to enhance industrial development and broaden the scope of applications in synthetic biology.

• 분석과학
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• 제28권3호
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• pp.228-235
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• 2015

본 연구는 지하수 중 라듐(²²⁶Ra) 분석을 위해 고상추출디스크(solid phase extraction disk)를 이용한 감마선분광분석법(이하 고상추출디스크법)을 제안하고 액체섬광계수기를 이용한 액체섬광계수(liquid scintillation counter, LSC)법 및 마리넬리비커(Marinelli beaker)를 이용한 감마선분광분석기(gamma ray spectrometer)법(이하 마리넬리비커법)과의 회수율 비교를 통해 적용성을 검토하였다. ²²⁶Ra을 회수한 고상추출디스크는 딸핵종의 방출을 방지하기 위해 폴리에틸렌 필름으로 밀봉 후 감마선분광분석기로 분석하였다. 24일 경과 후, ²²⁶Ra과 딸핵종인 ²¹⁴Bi과 ²¹⁴Pb이 방사평형 된 것으로 확인되었다. 라듐 표준물질을 이용하여 고상추출디스크법으로 분석한 딸핵종 ²¹⁴Bi와 ²¹⁴Pb의 회수율은 각각 80% (295.21 Kev)와 104% (351.92 Kev)로 액체섬광계수법보다 높게 나타났다. 바탕시료(blank) 측정시 감마선분광분석기 챔버내 질소를 주입했을 경우는 주입하지 않았을 경우보다 간섭치가 약 10% 이하로 낮아지는 것을 확인하였으며, 5 L 시료를 8만초 동안 측정한 검출한계는 0.17~0.40 pCi/L로 분석되어 미국 EPA 기준치인 1pCi/L를 만족하였다. 고상추출디스크법과 액체섬광계수법을 이용한 7개 지하수 시료 분석 결과, 두 방법의 상관계수(correlation coefficient)는 0.987로 나타나 추가적인 분석을 통해 통계적 유의성을 확보한다면 고상추출디스크법의 적용가능성이 높을 것으로 판단된다. 결과적으로, 고상추출디스크법을 이용한 지하수 중 ²²⁶Ra 농도 분석은 전처리 과정이 비교적 단순하여 분석시간이 절약되고 높은 회수율과 낮은 검출한계치 등의 장점을 가지고 있는 것으로 분석되었다. 또한 고상추출디스크법은 액체섬광계수법과 마리넬리비커법에 비해 많은 양의 시료를 전처리하기 쉽기 때문에 저준위 시료 분석에 유용할 것으로 판단된다.

• Bulletin of the Korean Chemical Society
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• 제31권8호
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• pp.2322-2328
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• 2010

A multiple solid-phase extraction (SPE) method was used with liquid chromatography, coupled with mass spectrometry (LC/MS), for the analysis of heterocyclic amines (HCAs) in human urine. Separation efficiencies based on the pH of the mobile phase and the types of columns were compared. An amide column showed better baseline separation and narrower HCA peak widths at pH 5.0 for the mobile phase than a $C_8$ column. Each SPE step, HLB, MCX, and HybridSPE, was optimized by controlling the pH conditions. The combined method with the three SPEs effectively removed interfering species that cause ion-suppression during HCA detection. Validation of the method, performed with SIM and SRM detection, showed correlation coefficients above 0.991 in the range 0.3 - 16.7 ng/mL. Recovery rates were 45.4 - 97.3% on the $C_8$ column and 71.8 - 101.4% on the amide column, and method detection limits were 0.11 - 0.65 ng/mL on the $C_8$ column and 0.12 - 0.48 ng/mL on the amide column. This method using multiple SPEs offers significant benefits for high-throughput determination of HCAs in urine.

• Bulletin of the Korean Chemical Society
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• 제24권10호
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• pp.1433-1436
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• 2003

A new method for the simultaneous determination of heavy metal ions in cigarette material by microwave digestion and reversed-phase high-performance liquid chromatography (RP-HPLC) has been developed. The cigarette material was digested by microwave digestion. Lead, cadmium, mercury, nickel and tin ions in the digested samples were pre-column derivatized with tetra-(2-chlorophenyl)-porphyrin ($T_2$-CPP) to form color chelates, which were then enriched by solid phase extraction with a $C_{18}$ cartridge. The chelates were separated on a Waters Xterra$^{TM}RP_{18}$ column by gradient elution with methanol (containing 0.05 mol/L pyrrolidine-aceticacid buffer salt, pH = 10.0) and acetone (containin0.05 mol/L pyrrolidine-acetic acid buffer salt, pH = 10.0)as mobile phase at a flow rate of 0.5mL/min and analyzed with a photodiode array detector from 350-600 nm. The detection limits of lead, cadmium, mercury, nickel and tin were 4,3,3,8 and 5 ng/L, respectively, in the original samples. This method was afforded good results.

• 한국축산식품학회지
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• 제28권5호
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• pp.637-644
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• 2008

식품 중 HCAs을 검출하기 위한 최적 전처리 방법을 확립하기 위해 가열 조리된 돼지고기 패티를 이용하여 서로 다른 4가지 SPE(solid-phase extraction)방법을 비교하였다. 4가지 전처리 방법을 통해 얻은 15가지 HCAs 회수율은 3.0%(방법 A, Tri-P-1)-74.7%(방법A, Tri-P-2)이었다. 그 중 $MeA{\alpha}C$가 평균적으로 73.4%로 가장 높은 회수율을 보였으며 Tri-MeIQx가 15.2%의 가장 낮은 회수율을 보였다. 4가지 전처리 방법 중 방법A와 방법D가 가장 높은 회수율과 검출빈도를 보였으며 방법B와 방법C는 Harman(14.8%)을 제외하고는 전혀 검출되지 않았고 회수율을 구할 수 없었다 발암 가능 물질인 IQ, $A{\alpha}C$, $MeA{\alpha}C$, Glu-P-1, Glu-P-2, MeIQ, MeIQx, PhIP 등을 검출하는 방법에는 방법A(48.7-74.6%)가 4가지 방법 중 가장 유리하다. HCAs는 극성에 따라 polar amines과 less-polar amines으로 구분할 수 있는데 방법A는 less-polar amines검출에 유리하고 방법D는 polar amines검출에 유리하다. 방법A와 방법D의 chromatogram을 비교한 결과 방법A와 방법D 모두 15가지 HCAs가 깨끗하게 분리되었지만 Tri-MeIQx 등을 검출하는데 방법A가 더욱 유리하다. SPE 전처리 방법 및 LC/MS 분석방법에 대한 유효성을 확인하기 위해 LOD(0.2-2.1 ng/mL)와 LOQ(0.8-9.7 ng/mL), 표준 편차(0.2-8.6)를 구하였다.

• Mass Spectrometry Letters
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• 제5권4호
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• pp.115-119
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• 2014

The Brazil nut (Bertholletia excelsa - Lecythidaceae) is considered a product with high economic value, being a food widely appreciated for its nutritional qualities. Although previous studies have reported the biochemical composition of Brazil nut oil, the knowledge regarding the phospholipid composition exhibits a disagreement: the composition of fatty acids present in the structures of phospholipids is reported as being different from the composition of the free fatty acids present in the oil. In this work, solid phase extraction (SPE) was employed to provide a fast extraction of the phospholipids from Brazil nuts, in order to compare the phospholipid profile of the in nature nuts and their fatty acids precursor present in the oil. The major phospholipids were characterized by mass spectrometry approach. Their fragmentation pattern through direct infusion electrospray ionization ion-trap tandem mass spectrometry ($ESI-IT-MS^2$) proved to be useful to unequivocal characterization of these substances. High resolution (HR) experiments through ESI using a quadruple time of flight mass spectrometry (QTOF) system were performed to reinforce the identifications.

• Bulletin of the Korean Chemical Society
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• 제34권11호
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• pp.3381-3386
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• 2013

This paper reports a method using molecularly imprinted polymers that are grafted onto the surface of carboxyl-modified multi-walled carbon nanotubes as the solid-phase extraction adsorbents to detect Rhodamine B in chili powder samples. The polymers were characterized by FTIR and TGA. Various parameters which probably influence efficiency of extraction were optimized. The analytical parameters such as precision, accuracy and linear working range were also determined in optimal experimental conditions. And the proposed method was applied to analysis of Rhodamine B in chili powder samples. The limits of detection and quantification were 2.57 and 8.56 ${\mu}g/g$, respectively. The recoveries for analytes were higher than 95% and relative standard deviation values were found to be in the range of 0.83-4.15%. This method was successfully applied for the determination of Rhodamine B.