• Mass Spectrometry Letters
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• v.5 no.1
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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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• v.2 no.1
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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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• v.30 no.1
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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.

• Analytical Science and Technology
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• v.28 no.3
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• pp.228-235
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• 2015

The efficiency and applicability of the solid phase extraction disk method in a ²²⁶Ra analysis were examined by the gamma ray spectrometer (GRS) method using a Marinelli beaker and the liquid scintillation counter (LSC) method for groundwater. The recovered ²²⁶Ra, which was filtered by the solid phase extraction disk, was analyzed using gamma ray spectrometer The disks, which were pretreated for caulking the daughter nuclide, were sealed with polyethylene film. Distilled water was used for the blank value of the ²²⁶Ra activity. The recovery values of ²¹⁴Bi and ²¹⁴Pb in the solid phase extraction disk, which used ²²⁶Ra standard material, were 80% (295.21 Kev) and 104% (351.92 Kev), respectively, which were higher than 75% determined by the LSC. The injection of nitrogen gas into the measuring chamber reduced the interference values by about 10%. The detection limits of the ²²⁶Ra activity in a blank sample of 5 L were 0.17~0.40 pCi/L after 80,000 seconds of measuring time. The relationship of the ²²⁶Ra activity in the solid phase extraction disk method and in the LSC method in seven groundwater samples showed a correlation coefficient value 0.987, which implies the applicability of the solid phase extraction disk method. The results showed that ²²⁶Ra activity in groundwater using the solid phase extraction disk method has the following benefits: simple pretreatment, time saving, high recovery values, a low detection limit, and so on. Compared with the LSC method and the GRS method using the Marinelli beaker for the ²²⁶Ra analysis, the solid phase extraction disk method could be useful in groundwater samples with low levels of activities of radionuclides because the method is not restricted by the volume of the sample.

• Bulletin of the Korean Chemical Society
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• v.31 no.8
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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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• v.24 no.10
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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.

• Food Science of Animal Resources
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• v.28 no.5
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• pp.637-644
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• 2008

Four different extraction and purification methods were evaluated to determine the heterocyclic amines (HCAs) in fried pork patties. Pork patties were cooked in the teflon-coated electric frying pan at $230^{\circ}C$ for 8 min per side. HCAs in the fried pork patties were extracted and purified using four different solid-phase extraction (SPE) methods and quantitated by LC-MS (API-ESI). Recovery of four different extraction and purification methods was evaluated by comparing the HCAs amounts quantified by the standard addition method. Validation of extraction and purification methods for fried pork patties was determined to establish accurate sample preparation. The recoveries of HCAs from different SPE methods were calculated. The recovery yields were 15.7-68.7% (Polar amine group) and 25.0-74.7% (less-polar amine group) in method A. Method D provided recovery yields ranging from 14.1% to 68.7% in polar amine groups and from 3.0% to 72.3% in less-polar amine groups, respectively. Modified procedures of Method A and D were the most suitable extraction and purification method for HCAs analysis from fried pork patties.

• Mass Spectrometry Letters
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• v.5 no.4
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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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• v.34 no.11
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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.

• Bulletin of the Korean Chemical Society
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• v.30 no.11
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• pp.2675-2679
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• 2009

This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.