• Bulletin of the Korean Chemical Society
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• v.27 no.6
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• pp.903-908
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• 2006

Various extraction procedures were investigated using reference materials and samples to evaluate extraction efficiency and effectiveness. Inductively coupled plasma mass spectrometry (ICP-MS) was used to measure total arsenic and to quantitate arsenic species when coupled to an HPLC (high pressure liquid chromatography). Arsenic species were extracted from rice flour (NIST SRM 1568a) with water/methanol mixtures using accelerated solvent extraction (ASE). Total arsenic extraction efficiency ranged from 42 to 64%, for water and various methanol concentrations. From spinach (NIST SRM 1570), freeze-dried apple, and rice flour (NIST SRM 1568a), arsenic species were extracted with trifluoroacetic acid (TFA) at 100 ${^{\circ}C}$. Total arsenic extraction efficiency was 90% for spinach, 75% for freeze-dried apple, and 83% for rice flour. Enzymatic extraction with alpha-amylase and sonication resulted in extraction efficiency of 104% for rice flour, 98% for freeze-dried apple, and 7% for spinach. Chromatograms of arsenic species extracted by the optimum extraction methods were obtained, and the species were quantified. Arsenite (As(III)), arsenate (As(V)), dimethylarsinic acid (DMA), and monomethylarsonic acid (MMA) were found in the apple sample, and DMA and As(V) in the rice flour sample. As(V) and MMA were found in three herbal dietary supplement samples.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.45 no.3
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• pp.211-215
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• 2000

Lipid extraction preceding fatty acid methyl esters preparation for gas-liquid chromatography is time-consuming and cumbersome. We performed one-step extraction/methylation method with a mixture of methanol-heptane-benzene-DMP-H$_2$SO$_4$ without prior fat extraction. The simultaneous digestion and lipid transmethylation takes place at 8$0^{\circ}C$ in a single phase. After cooling till room temperature, two phases are formed. The upper one of the phases contains the fatty acid methyl esters ready for GLC. The fatty acid composition of major industrial crops obtained by the one step extraction/methylation method (method 1 and 2) was almost identical with the fatty acid composition of the pure fats extracted with hexane by the Soxtec instrument (method 3). Due to its simplicity, speed, and reduced organic solvent the one-step extraction/methylation method (method 1 and 2) should be useful to determine overall fatty acid composition, especially in situations where many samples have to be analyzed.

• Food Science of Animal Resources
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• v.35 no.6
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• pp.765-771
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• 2015

The development of a sample preparation method and optimization of the analytical instrumentation conditions were performed for the determination of the vitamin B₁₂ content in emulsified baby foods sold on the Korea market. After removal of the milk protein and fats by chloroform extraction and centrifugation, the vitamin B₁₂ was water extracted from the sample. Following filtration of the solution through a nylon filter, the water-soluble extract was purified by solid-phase extraction using a Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS). The solution eluted from the cartridge was dried under a stream of nitrogen gas and reconstituted with 1 mL of water. The sample solution was injected into an LC-MS/MS system after optimizing the mobile phase for vitamin B₁₂ detection. The calibration curve showed good linearity with the coefficient of correlation (r²) value of 0.9999. The limit of detection was 0.03 µg/L and the limit of quantitation was 0.1 µg/L. The method of detection limit was 0.02 µg/kg. The vitamin B₁₂ recovery from a spiking test was 99.62% for infant formula and 99.46% for cereal-based baby food. The sample preparation method developed in this study would be appropriate for the rapid determination of the vitamin B₁₂ content in infant formula and baby foods with emulsified milk characteristics. The ability to obtain stable results more quickly and efficiently would also allow governments to exercise a more extensive quality control inspection and monitoring of products expected to contain vitamin B₁₂. This method could be implemented in laboratories that require time and labor saving.

• Journal of the Korean Society of Food Science and Nutrition
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• v.39 no.9
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• pp.1249-1256
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• 2010

Forty natural plants collected in Jeju, Jeonnam-Goheung, and Gyeongbuk-Ulleung were extracted using a pressurized liquid. Extraction yields of total soluble solids and total phenolics (TP), and integral antioxidative capacity (IAC) were measured, and antimicrobial activity was tested against Streptococcus parauberis, Streptococcus iniae, Edwardsiella tarda, and Vibrio ordalii. Jipsinnamul showed the highest content of TP (174.4 mg GAE/g), followed by Mulchamnamu (116.9), Seoeonamu (113.3), and Buknamu (108.2). Percent TP/TSS was high in Jipsinnamul (72.6%), Seoeonamu (47.3%), Mulchamnamu (46.4%), Jageumu (40.2%), and Baneulkkot (40.1%), respectively. Magamok, Nadosongipul, Buknamu, Mulchamnamu, and Seoeonamu showed 5.81, 3.96, 3.63, 3.63, and 3.34 mmol ascorbic acid equivalents/g of IAC of water-soluble substances, and Seoeonamu, Magamok, Seipijilpul, Mulchamnamu, Baneulkkot, and Seomgirincho showed 8.51, 6.57, 5.68, 3.85, 3.83, and 3.69 mmol Trolox equivalents/g of IAC of lipid-soluble substances, respectively. Only nine species such as Baneulkkot, Dokhwal, Jipsinnamul, Mulchamnamu, Nadosongipul, Seipijilpul, Seoeonamu, Seomgirincho, and Sumbadi of 40 selected plants showed the antimicrobial activity against four bacteria tested. Jipsinnamul showed the strong antimicrobial activity against S. iniae, while Dokhwal, Nadosongipul, and Sumbadi against S. parauberis and S. iniae, and Mulchamnamu, Seoeonamu, and Seipijilpul against V. ordalii.

• Analytical Science and Technology
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• v.23 no.6
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• pp.524-530
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• 2010

Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.

• Journal of Applied Biological Chemistry
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• v.59 no.4
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• pp.331-336
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• 2016

Analytical methods for methiozolin in soil, water and turfgrass were established and dissipation patterns of methiozolin in soil and turfgrass were elucidated. Analysis was done using a high performance liquid chromatography with an ultra violet detector at the wavelength of 280 nm after extraction with acetone, liquid-liquid partition with dichloromethane, and a solid phase extraction purification. Limit of determination and Limit of quantitation were 1.0, 0.5, 1.0 ng, and 0.001, 0.1, 0.01 mg/kg for water, turfgrass, and soil, respectively. Recovery rates of methiozolin from soil, water, and turfgrass were ranged 87.5~111.3, 92.8~97.4, and 78.2~98.5 %, respectively. The turfgrass and soil samples were collected at 0, 1, 4, 7, 14, 30, 45, and 60 after spray on green area in golf course. Residues of methiozlolin were not translocated to lower soil layer but detected only in turfgrasses and root area of turfgrass. Half-lives of methiozolin in turfgrass were 10.7 days and 8.8 days in soil from root area.

• Proceedings of KOSOMES biannual meeting
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• 2007.05a
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• pp.21-26
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• 2007

The Protocol adopted in Sep. 1997 included the new Annex VI of MARPOL 73/78, which entered into force on 19 May 2005. Revision for the accept MARPOL Annex VI with make public on 29 Dec. 2005 and enforce on 29 Jun. 2006. For all that not installation at oil terminal or if installed do not used. The purpose of this study is to research and evaluate the methods of sampling and analysis, and the pollution measure of existed VOCs during the bulk liquid cargo operation at vessels. As the sampling instrument of VOCs, Tedlar bag has the effect of decrease in concentration by the chemical reaction and absorption, and the method using the solvent extraction has error cause because of the extraction, the absorption tube has error by the breakthrough. But canister is the best sampling instrument because of having no sampling mistake. The study on VOCs emission is not sufficient for the research on the pollution cause and the analysis data on the HAP during the bulk liquid cargo operation at vessels. Hence, monitoring on the management hazardous VOCs need to be continued during the cargo operation at vessels and VOCs management field must be study for the make progress at a good pace for reason of crew's health.

• Journal of Environmental Science International
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• v.2 no.1
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• pp.61-72
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• 1993

Result of this study indicate that two criteria must be met in order to have effective macrocycle-mediated transport in these emulsionsystem. First, one must effective extraction of the post transition metals, $Cd^{2+}$. $Pb^{2+}$ and $Hg^{2+}$ , into toluene membrane. The effectiveness of this extraction is greatest if log K values for the metal-macrocycle interaction is large. Second, the ratio of the log K values for the metal ion-receiving phase to the metal ion-macrocycle interaction must be large enough to ensure quantitative stripping of the metal ion at the toluene phase interface. Control of the first step can be obtained by appropriate selection of macrocycle donor atom, substituents, and cavity radius. The second step can be controlled by selecting the proper complexing agent for inclusion in the receiving phase. The order of the transport, when using the several $A^-$ species such as $SCN^-$, $1^-$, $Br^-$ and $Cl^-$ is the order of the changing degree of solvation for $A^-$ and the transport of the metals is also affected by the control of concentration for receiving species because of solubility-differences. In this study, we can seperate each single metal ion from the mixture of $Cd^{2+}$, $Pb^{2+}$, and $Hg^{2+}$ ions by using the toluene membranes controlled by optimized conditions. Transport of the single metal is also very good, and alkaline and alkaline earth metals as interferences ions did not affect the seperation of the metals in this macrocycle-liquid membrances but transition metal ions were partially affected as interferences for the post transition metal ions.

• Mass Spectrometry Letters
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• v.8 no.2
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• pp.39-43
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• 2017

Meldonium is a drug for treating ischemia by expanding the arteries but it can also enhance the performance of sports players. The World Anti-Doping Agency (WADA) has included it in the list of prohibited substances since 2016. Meldonium is one of the challenging substances for anti-doping testing because it is difficult to recover by general liquid-liquid or solid phase extraction due to its permanent charge and high polarity. Therefore, high-performance liquid chromatography (HPLC) is currently used by injecting a diluted urine sample (known as the "dilute-and-shoot" strategy). There is no loss of target compounds in the extraction/cleanup procedure but its high matrix effect could interfere in their separation or detection from the endogenous urinary compounds. We report a single method using high-resolution mass spectrometry that can be used for both screening and confirmation, which follows the "dilute-and-shoot" strategy. In this method, the endogenous compounds' interfering peaks in the mass spectrum are separated at a high resolution of FWHM 140,000, and the results are suitable for substance detection following the WADA guidelines. The interferences in the obtained mass spectrum of the urine matrix are identified as acetylcholine, lysine, and glutamine by further analysis and database searching. Validation of the method is performed in routine anti-doping testing, and the limit of detection is 50 ng/mL. This method uses simple sample preparation and a general reverse phase HPLC column, and it can be easily applied to other substances.

• Korean Chemical Engineering Research
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• v.60 no.4
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• pp.473-477
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• 2022

In this study, candidate technologies for lithium recovery from the process waste liquid generated in the waste battery recycling process were reviewed, and technologies applicable to the process from the commercialization point of view were reviewed from a qualitative point of view. The evaporation method is difficult to apply because it requires a large-scale land and shows a low recovery rate due to the loss of Li during the concentration process. In the case of precipitation, a commercially available technology shows a high recovery rate due to the high Li/Na selectivity of phosphoric acid, but there are disadvantages in that the process is complicated due to the use of expensive phosphoric acid, requiring a recovery step, and continuous operation is impossible because solids are handled in the Li concentration process. In the case of solvent extraction, if we find an inexpensive extractant with high Li/Na selectivity, continuous operation is possible with the method used in extraction of other metals in the previous step, and when Li is concentrated, continuous operation is possible because it is in a liquid state. If it shows a similar recovery rate compared to precipitation technology, commercialization will be the most likely.