• Korean Journal of Clinical Laboratory Science
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• v.55 no.4
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• pp.261-268
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• 2023

[¹⁸F]Fluorocholine is a radiopharmaceutical used non-invasively in positron emission tomography to diagnose parathyroid adenoma, prostate cancer, and hepatocellular carcinoma by evaluating the choline metabolism. In this study, a radiolabeling method for [¹⁸F]fluorocholine was optimized using a solid phase extraction (SPE) cartridge. [¹⁸F]Fluorocholine was labeled in two steps using an automated synthesizer. In the first step, dibromomethane was reacted with [¹⁸F]KF/K2.2.2/K₂CO₃ to obtain the intermediate [¹⁸F]fluorobromomethane. In the second step, [¹⁸F]fluorobromomethane was passed through a Sep-Pak^Ⓡ Silica SPE cartridge to remove the impurities and then reacted with N,N-dimethylaminoethanol (DMAE) in a Sep-Pak^Ⓡ C18 SPE cartridge to label [¹⁸F]fluorocholine. The reaction conditions of [¹⁸F]fluorocholine were optimized. The synthesis yield was confirmed according to the number of silica cartridges and DMAE concentration. No statistically significant difference in the synthesis yield of [¹⁸F]fluorocholine was observed when using four or three silica cartridges (P>0.05). The labeling yield was 11.5±0.5% (N=4) when DMAE was used as its original solution. On the other hand, when diluted to 10% with dimethyl sulfoxide, the radiochemical yield increased significantly to 30.1±5.2% (N=20). In conclusion, [¹⁸F]Fluorocholine for clinical use can be synthesized stably in high yield by applying an optimized synthesis method.

• YAKHAK HOEJI
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• v.46 no.6
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• pp.392-397
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• 2002

A simple and sensitive high performance liquid chromatographic method to quantitate ursodeoxycholic acid in crude drug pharmaceuticals was investigated. Ursodeoxycholic acid react with 2-bromoacetyl-6-methoxynaphthalene (Br-AMN) in the presence of triethylamine to form highly fluorescent derivative. The derivatization procedure was performed at 7$0^{\circ}C$ and completed within 30 min. The optimal wavelength of the fluorescence detector are λ$_{ex}$=300 nm and λ$_{em}$ = 460 nm. The LOD of the ursodeoxycholic acid was 25 ng/mι based on the S/N =3, and the LOQ was 80 ng/mι based on S/N = 10. Crude drug pharmaceuticals pretreated by solid phase extraction (Sep-pak $C_{18}$ cartridge) which were shown very good separation and recovery values for the compound.d.

• Mass Spectrometry Letters
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• v.13 no.4
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• pp.158-165
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• 2022

Many therapeutic class drugs such as beta-blocker, corticosteroids, NSAIDs, etc are prohibited substances in the horse racing industry. Liquid chromatography-tandem mass spectrometry (LC-MS/MS) technology makes it possible to isolate drugs from interference, enables various drug analyses in complex biological samples due to its sensitive sensitivity, and has been successfully applied to doping control. In this paper, we describe a rapid and sensitive method based on solid-phase extraction (SPE) using solid phase cartridge and LC-MS/MS to screen for different class's 35 drug targets in equine plasma. Plasma samples were pretreated by SPE with the NEXUS cartridge consisted non-polar carbon resin and minimum buffer solvent. Chromatographic separation of the analytes was performed on ACQUITY HSS C18 column (2.1 × 150 mm, 1.8 ㎛). The elution gradient was conducted with 5 mM ammonium formate (pH 3.0) in distilled water and 0.1% formic acid in acetonitrile at a flow rate of 0.25 mL/min. The selected reaction monitoring (SRM) mode was used for drug screening with multiple transitions in the positive ionization mode. The specificity, limit of detection, recovery, and stability was evaluated for validation. The method was found to be sensitive and reproducible for drug screening. The method was applied to plasma sample analysis for the proficiency test from the Association of Racing Chemist.

• Journal of Korean Society on Water Environment
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• v.25 no.5
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• pp.720-726
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• 2009

We investigated the most effective pre-treatment processes and LC/MS/MS condition for microcystins analysis. With a step-by-step pre-treatment, efficiencies of several established methods were compared. At the level of cell burst, sonication method was found to be the most efficient. As a mycrocystins first extraction solvent, 5% acetic acid showed the highest efficiency. An isolation and recovery rate of mycrocystins of ODS Sep-Pak $C_{18}$ cartridge was higher than HLB SPE cartridge. As a final elution solvent from cartridge, 100% MeOH had a better efficiency than others. Using a LC/MS/MS, effective analytical methods were established. C18 reverse column was used and gradient elution was performed with using acetonitrile, 0.1% formic acid as a mobile phase. We analysed to 0.8 mL/min flow rate fit to the $5{\mu}m$ particle size column and $55^{\circ}C$ housing temperature. The validity of established analytical method was evaluated that MDL as average $0.050{\pm}0.014{\mu}g/L$ and LOQ as average $0.160{\pm}0.045{\mu}g/L$ had a good sensitivity over 40 magnification rather than $2{\mu}g/L$ detection limit of HPLC.

• Analytical Science and Technology
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• v.23 no.5
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• pp.437-445
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• 2010

The aim of this study was to develop an analytical method for sulfonamide antibiotics (sulfadiazine, sulfamerazine, sulfamethazine, sulfamethoxazole, sulfathiazole) and their metabolites ($N^4$-acetylsulfadiazine, $N^4$-acetylsulfamerazine, $N^4$-acetylsulfamethazine, $N^4$-acetylsulfamethoxazole, sulfamethoxazole-$N^1$-glucuronide) in environmental samples. The solid phase extraction (SPE) with LC/ESI-MS/MS have been used for the analysis of target compounds, and the recoveries of SPE clean-up were at the range of 12-94% for C18 cartridge, 60-95% for HLB cartridge, 25-123% for MCX cartridge, and 70-90% for tandem HLB/MCX. By established method, detection limit, recovery, and relative standard deviation were 0.001~0.187 ng/mL, 66~115%, and 5~17%, respectively. This method was effective and sensitive to use for the simultaneous determination of sulfonamide antibiotics and their metabolites in environmental samples. Four sulfonamide antibiotics were detected at the range of 0.008~2.153 ng/mL. For metabolites, only $N^4$-acetylsulfamethoxazole was detected, but the concentration was under the MDL level.

• Bulletin of the Korean Chemical Society
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• v.28 no.2
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• pp.276-280
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• 2007

In this work, caffeine and some catechin compounds + C, EC, EGC, and EGCG were extracted from green tea by using molecular imprinted polymers (MIP) as sorbent materials in a solid-phase extraction (SPE) process known as MISPE (molecular imprinted solid-phase extraction). For synthesis of MIP, caffeine was employed as the template, MAA as the monomer, EGDMA as the crosslinker, and AIBN as the initiator. A solution of caffeine (0.2 mg/mL in methanol) was utilized in the solid extraction cartridges following loading, washing, and elution procedures with acetonitrile, methanol, and methanol-acetic acid (90/10, %v/v) as the solvents, respectively. This solid-phase extraction protocol was applied for the extraction of caffeine and some catechin compounds from green tea. A comparison was made between the results obtained with the MIP cartridges and a traditional C18 reversed-phase cartridge. It was thereupon found that the recovery of caffeine by the MIPbased sorbent used in this work was almost two and four times greater than that by a commercially available C18 material. A quantitative analysis was conducted by high performance liquid chromatography (HPLC) using a C18 column (5 μm, 250 × 4.6 mm) with methanol/water (40/60, %v/v) as the mobile phase at a flow rate of 0.5 mL/min.

• Korean Journal of Environmental Agriculture
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• v.23 no.4
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• pp.251-257
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• 2004

Analytical methods were developed to determine cyclosulfamuron residues in soil, water, rice grain and straw using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. In these methods, cyclosulfamuron was extracted with aqueous $Na_2HPO_4$/acetone and acetone/methanol mixture from soil and rice samples respectively. Liquid-liquid partition coupled with ion-associated technique, Florisil column chromatography, and solid-phase extraction (SPE) were used to separate cyclosulfamuron from interfering co-extractives prior to HPLC analysis. For water sample, the residue was enriched in $C_{18}$-SPE cartridge, cleaned up in situ, and directly subjected to HPLC. Reverse-phase HPLC under ion-suppression was successfully applied to determine cyclo-sulfamuron in sample extracts with the detection at its ${\lambda}_{max}$ (254 nm). Recoveries from fortified samples averaged $87.8{\pm}7.1%$ (n=12), $97.3{\pm}7.2%$ (n=12), $90.8{\pm}6.6%$ (n=6), and $78.5{\pm}6.7%$ (n=6) for soil, water, rice grain and straw, respectively. Detection limits of the methods were 0.004 mg/kg, 0.001 mg/L, 0.01 mg/kg and 0.02 mg/kg for soil, water, rice grain and straw samples, respectively.

• Food Science and Biotechnology
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• v.18 no.2
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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.

• The Korean Journal of Nuclear Medicine Technology
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• v.22 no.1
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• pp.51-54
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• 2018

Purpose $^{18}F-THK5351$ is the newly developed PET probe for tau imaging in alzheimer's disease. The purpose of study was to establish the automated production of $^{18}F-THK5351$ on a commercial module. Materials and Methods Two different approaches were evaluated for the synthesis of $^{18}F-THK5351$. The first approach (method I) included the nucleophilic $^{18}F$-fluorination of the tosylate precursor, subsequently followed by pre-HPLC purification of crude reaction mixture with SPE cartridge. In the second approach (method II), the crude reaction mixture was directly introduced to a semi-preparative HPLC without SPE purification. The radiosynthesis of $^{18}F-THK5351$ was performed on a commercial GE $TRACERlab^{TM}$ $FX-_{FN}$ module. Quality control of $^{18}F-THK5351$ was carried out to meet the criteria guidelined in USP for PET radiopharmaceuticals. Results The overall radiochemical yield of method I was $23.8{\pm}1.9%$ (n=4) as the decay-corrected yield (end of synthesis, EOS) and the total synthesis time was $75{\pm}3min$. The radiochemical yield of method II was $31.9{\pm}6.7%$ (decay-corrected, n=10) and the total preparation time was $70{\pm}2min$. The radiochemical purity was>98%. Conclusion This study shows that method II provides higher radiochemical yield and shorter production time compared to the pre-SPE purification described in method I. The $^{18}F-THK5351$ synthesis by method II will be ideal for routine clinical application, considering short physical half-life of fluorine-18 ($t_{1/2}=110min$).

• Archives of Pharmacal Research
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• v.28 no.4
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• pp.463-468
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• 2005

The purpose of the present study was to develop a standard protocol for imidapril hydrochloride bioequivalence testing. For this reason, a specific LC-MS method was developed and validated for the determination of imidapril in human plasma. A solid-phase extraction cartridge, $Sep-pak^{R}$ C18, was used to extract imidapril and ramipril (an internal standard) from deproteinized plasma. The compounds were separated using a XTerra $MS^{R}$?C18 column ($3.5 {\mu}m, 2.1\times150 mm$) and $acetonitrile-0.1\%$ formic acid (67:33, v/v) adjusted to pH 2.4 by 2 mmol/L ammonium formic acid, as mobile phase at 0.3 mL/min. Imidapril was detected as m/z 406 at a retention time of ca. 2.3 min, and ramipril as m/z 417 at ca. 3.6 min. The described method showed acceptable specificity, linearity from 0.5 to 100 ng/mL, precision (expressed as a relative standard deviation of less than $15\%$), accuracy, and stability. The plasma concentration-versus-time curves of eight healthy male volunteers administered a single dose of imidapril (10 mg), gave an $AUC_{12hr}$ of imidapril of $121.48\pm35.81 ng mL^{-1} h$, and $C_{max} and T_{max}$ values of $32.59\pm9.76 ng/mL and 1.75\pm0.27 h$. The developed method should be useful for the determination of imidapril in plasma with sufficient sensitivity and specificity in bioequivalence study.