• 분석과학
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• 제23권4호
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• pp.395-404
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• 2010

레몬과 콩 그리고 채소류에서 105개의 잔류농약을 다종 다성분 분석법으로 GC/MS/MS 분석하였다. 각 시료로부터 acetonitrile로 1차 추출하고 NaCl 15 g을 첨가한 다음 액-액 분배하였으며, Florisil 고체상(SPE) Cartridge로 정제하여 분석하였다. 레몬과 콩에서의 105개 농약의 회수율은 azinphos-methyl, famoxadone, fenamidone, flufenoxuron, triadimefon을 제외한 모든 농약에서 우수한 것으로 나타났는데 레몬에서 71.1~126.0%, 콩에서는 72.5~124.5% 였다. 또한 레몬에서의 검출한계와 정량한계는 각각 0.001~150 ng/mL와 0.004~500 ng/mL으로 확인되었다.

• 농업생명과학연구
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• 제46권6호
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• pp.165-171
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• 2012

As a preceding study for investigating the influence of sound wave stimulus on Arabidopsis thaliana metabolomics, the polar secondary metabolomes of the plant were determined using high performance liquid chromatography coupled with tandem mass spectrometry. A total of 10 polar secondary metabolomes were characterized and quantified. Among them, 4 metabolomes, p-coumaroylagmatine isomer (7 and 8), p-coumaroylagmatine isomer (9 and 10) were identified in the plant for the first time. The validation was conducted in terms of linearity, recovery, precision, limit of detection (LOD) and limit of quantification (LOQ). The validated method was applied to the simultaneous quantification of the 10 polar secondary metabolomes.

• 분석과학
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• 제34권4호
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• pp.153-159
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• 2021

In this study, we describe the development of a new high-performance liquid chromatography (HPLC) method for the simultaneous analysis of six bioactive compounds (including gallic acid, epicatechin 3-gallate, quercitrin, afzelin, quercetin, and kaempferol) from Orostachys japonicus. The extraction method was investigated and optimization of the extraction time (min), solvent composition (%), and solvent to material ratio were conducted. As a result, 30 min extraction with 50% methanol and 40:1 mL/g of solvent: material ratio achieved the highest extraction efficiency with a yield of 3.32 mg/g. Furthermore, the developed HPLC method was validated and the correlation coefficient (R) values were within the satisfactory range of 0.9995-0.9999 over the linearity range of 1.53-417 ㎍/mL. The limit of detection and limit of quantification for the six active components were between 0.03-0.08 ㎍/mL and 0.08-0.26 ㎍/mL, respectively. With these newly optimized and developed methods, four batches of O. japonicus were analyzed to confirm the high extraction efficiency of the method and the feasibility of an application.

• 한국식품과학회지
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• 제53권6호
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• pp.682-687
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• 2021

The purpose of this study was to validate a high-performance liquid chromatography (HPLC) method for the quantitative analysis of quercetin in various foods. The method was based on HPLC-UV (360 nm). The method was validated using candy, beverage, and sausage which were tested for specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy, and the measurement uncertainty was assessed. Matrix-matched calibration was also applied. The calibration curves (0.5-50 mg/L) showed good linearity (r²≥0.9998). LOD and LOQ ranged from 0.15 to 0.31 mg/kg and from 0.44 to 0.93 mg/kg, respectively. The average accuracy and precision at 0.5, 2.5, and 10 mg/kg ranged from 84.3 to 102.0% and 0.7 to 3.0 relative standard deviation (RSD%), respectively. This study confirmed the applicability of the proposed method by applying it to commercial products, such as teas and beverages. Thus, the proposed analytical method is suitable for quantifying quercetin in various foods.

• 한국수산과학회지
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• 제43권4호
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• pp.293-297
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• 2010

To prevent amnesic shellfish poisoning (ASP) resulting from the consumption of shellfish contaminated with domoic acid, the quantitative analysis of domoic acid is very important. We validated a high performance liquid chromatography (HPLC) method for accurate and precise quantification of domoic acid. A clear peak and the isolation of domoic acid resulted on injecting a 50% methanol extract of CRM-ASP-Mus-c mussel reference material using HPLC. The limit of detection of domoic acid under the established HPLC conditions was $0.10\;{\mu}g/g$, and the limit of quantification of the toxin under the same conditions was $0.25\;{\mu}g/g$. The intra-accuracy and precision for domoic acid in CRM-ASP-Mus-c were 90.7-95.7% and 0.28-22.25%, respectively. The inter-accuracy and precision for domoic acid were 89.1-97.1% and 1.7-4.1%, respectively. The mean recovery of domoic acid in methanol extracts from ten species of marine invertebrates was 88.6-1105.1%.

• 대한수의학회지
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• 제48권1호
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• pp.9-16
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• 2008

A method for the quantification of eugenol in the medicinal herb Clove was developed and validated. For preparation of sample solutions clove was dried at $60^{\circ}C$ for 2h and ground by mixer and extracted with 95% ethanol for shaking extraction. The elutes were analyzed by HPLC system included a reversed phase column, a isocratic mobile phase of 60% methanol and PDA detector set at 280 nm. Calibration graphs were linear with very good correlation coefficients ($r^2>0.9999$) from $0.0125~1{\mu}g/ml$. The limit of detection per sample injection ($20{\mu}l$) was $0.81ng/{\mu}l$ and limit of quantification was $2.47ng/{\mu}l$. The method showed good intra-day precision (%RSD 0.08 ~ 0.27%) and inter-day precision (%RSD 0.32 ~ 1.19%).

• 한국어병학회지
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• 제34권2호
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• pp.261-269
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• 2021

This study presents the evaluation of sample extraction and purification procedure for the determination of residues of febantel and its metabolites, fenbendazole, oxfendazole and oxfendazole sulfone in rockfish (Sebastes schlegeli) muscle using liquid chromatography-tandem mass spectrometry. Residues of febantel and its metabolites in rockfish muscle were analyzed using each different sample preparation method from Korean Food Standards Codex (KFSC), Food Safety and Inspection Service (FSIS, USA), and the modified FSIS method using QuEChERS kit (FSIS-Q), respectively. Each method was compared for mean recoveries and repeatabilities. Since FSIS-Q showed higher repeatabilities (coefficient of variation, CV of 2.4%~10.9%) than those of FSIS method (CV of 4.6%~17.5%), recoveries from FSIS-Q were compared with those from KFSC method. FSIS-Q showed significantly higher recoveries of 83.1%~110.1% (P < 0.05) than those from KFSC method of 64.7%~107.4%. In addition, FSIS-Q showed a good linearity over the range of 2.5~200 ㎍/kg, and excellent sensitivities with limit of detection of 0.46~0.71 ㎍/kg and limit of quantification of 1.08~2.15 ㎍/kg. Although all the sample preparation methods turned out to be able to meet CODEX guideline for all the compounds, FSIS method and FSIS-Q validated in this study could be applied to screening and quantification for residues of febantel and its metabolites in rockfish muscle with efficient preparation procedures.

• 한국동물위생학회지
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• 제45권3호
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• pp.243-248
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• 2022

The HPLC conditions for analysis of ivermectin in solutions dosage forms of commercial anthelmintics are different for each product. The purpose of this study was to establish a standardized chromatographic method for the quantification of ivermectin in solution. The separation was achieved on Waters Xbridge C18 column (4.6×150 nm, 5 ㎛) using different kinds of mobile phase composed of water/methanol/acetonitrile (15/34/51, v/v and 19.5/27.5/53, v/v), with UV detection at wavelengths 245 nm and 254 nm. A total of five commercial ivermectin in solution samples were analyzed. In this study, the optimal chromatographic conditions for analysis of ivermectin in solution were mobile phase of water/methanol/acetonitrile (15/34/51, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 245 nm using a Waters Xbridge C18 column (4.6×250 nm, 5 ㎛) at a column temperature of 25℃. The linearity was observed in the concentration range of 50~150 ㎍/mL, with a correlation coefficient, r²= 0.99999. The limit of detection and the limit of quantification were 0.88 and 2.68 ㎍/mL, respectively. The accuracy (% recovery) was found to be 98.9 to 100.3%. Intra-day and Intermediate precisions with relative standard deviations were less than 1.0%. The content of ivermectin for five market samples ranged 91.2~102.7%. The proposed method was also found to be robust, therefore, the method can be used for the routine analysis of ivermectin in solutions dosage forms.

• Mass Spectrometry Letters
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• 제13권1호
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• pp.20-25
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• 2022

Fargesin, a tetrahydrofurofuranoid lignan isolated from Flos Magnoliae, shows anti-inflammatory, anti-oxidative, anti-allergic, and anti-hypertensive activities. To evaluate the pharmacokinetics of fargesin in mice, a sensitive, simple, and selective liquid chromatography-high resolution mass spectrometric method using electrospray ionization and parallel reaction monitoring mode was developed and validated for the quantification of fargesin in mouse plasma. Protein precipitation of 6 µL mouse plasma with methanol was used as sample clean-up procedure. The standard curve was linear over the range of 0.2-500 ng/mL in mouse plasma with the lower limit of quantification level at 0.2 ng/mL. The intra- and inter-day coefficient variations and accuracies for fargesin at four quality control concentrations including were 3.6-11.3% and 90.0-106.6%, respectively. Intravenously injected fargesin disappeared rapidly from the plasma with high clearance values (53.2-55.5 mL/min/kg) at 1, 2, and 4 mg/kg doses. Absolute bioavailability of fargesin was 4.1-9.6% after oral administration of fargesin at doses of 1, 2, and 4 mg/kg to mice.

• Mass Spectrometry Letters
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• 제4권3호
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• pp.55-58
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• 2013

Dioscin is a biologically active steroidal saponin with anticancer and hepatoprotective effects. A rapid, selective, and sensitive liquid chromatographic method with electrospray ionization tandem mass spectrometry was developed for the quantification of dioscin in rat plasma. Dioscin was extracted from rat plasma using ethyl acetate at acidic pH. The analytes were separated on a Halo C18 column using gradient elution of acetonitrile and 0.1% formic acid and detected by tandem mass spectrometry in selected reaction monitoring mode. The standard curve was linear ($r^2$ = 0.998) over the concentration range of 1-100 ng/mL. The lower limit of quantification was 1.0 ng/mL using 50 ${\mu}L$ of plasma sample. The coefficient of variation and relative error for intra- and inter-assay at four QC levels were 1.3 to 8.0% and -5.4 to 10.0%, respectively. This method was applied successfully to the pharmacokinetic study of dioscin after oral administration of dioscin at a dose of 29.2 mg/kg in male Sprague-Dawley rats.