• Analytical Science and Technology
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• v.36 no.1
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• pp.32-43
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• 2023

This study reports for the first time about a stability indicating RP-HPLC method for qualitative and quantitative determination of acalabrutinib in bulk and dosage form and in presence its impurities 1, 2 and 3. The chromatographic separation was carried on Zorbax XDB-C18 (250×4.6 mm; 5 µ id) as stationary phase, Phosphate buffer pH 6.4 and methanol 80:20 (v/v) as mobile phase at a flow rate of 1.0 mL/min, UV detection was carried at wavelength of 238 nm and the analysis was completed with a run time of 15 min. In these conditions the retention time of acalabrutinib and its impurities 1, 2 and 3 was observed to be 3.50, 4.83, 8.40 and 9.93 min respectively. The method was validated for system suitability, range of analysis, precision, specificity, stability and robustness. Spiked recovery at 50 %, 100 % and 150 % was carried for both standard and impurities and the acceptable % recovery of 98-102 was observed for acalabrutinib and both impurities studied and the % RSD in each spiked level was found to be less than 2. Stability tests were done through exposure of the analyte solution to five different stress conditions i.e expose to 1N hydrochloric acid, 1 N sodium hydroxide, 3 % peroxide, 80 ℃ temperature and UV radiation at 254 nm. In all the degradation condition, standard drug acalabrutinib was detected along with both the impurities studied and the degradation products were successfully separated. In the formulation analysis there is no other chromatographic detection of other impurities and formulation excipients. Hence the developed method was found to be suitable for the quantification of acalabrutinib and can separate and analyse impurities 1 and 2.

• Korean Journal of Food Science and Technology
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• v.36 no.4
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• pp.558-562
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• 2004

Conditions for rapid quantification of isoflavones were studied. Rapid and clear separation of isoflavones (genistin and daidzin) was obtained using solvent system of chloroform : methanol : water : acetic acid (60 : 30 : 10 : 0.5, v/v/v/v). Quantification of each isoflavone separated by TLC was conducted by densitometry analysis. Genistin and daidzin were quantified in $0.15-1.80\;{\mu}g/{\mu}L$ range with 99% confidence. Concentrations of isoflavones in soybeans and kudzu roots originated from Korea were determined, and validity of TLC method for quantification of isoflavones was confirmed by comparison with HPLC analysis.

• Analytical Science and Technology
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• v.30 no.5
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• pp.226-233
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• 2017

In general, quantitative chemical analysis in various areas including food, the environment, in vitro diagnostics, etc., requires traceability in order to increase the reliability of the measurements. Measurement traceability is a property of an unbroken chain of comparisons relating an instrument's measurements to SI units. Purity analysis is the first process for establishing traceability to SI units in chemical measurements. The purpose of this study is to develop and validate a method of purity assignment for establishing the traceability of $17{\beta}$-estradiol measurements in an in vitro diagnostics field. The establishment of this method is very important as it can be applied to the development of CRM and to the analysis of the purity of other hormones. The method of assignment of the purity of $17{\beta}$-estradiol was developed using the mass balance method and was validated through participation in an International comparison. In the mass balance method, impurities are categorized into four classes as follows: total related structure impurities, water, residual organic solvents, and nonvolatiles/inorganics. In this study, total related structure impurities were characterized by a gas chromatography-flame ionization detector (GC-FID) and a high-performance liquid chromatography-ultraviolet (HPLC-UV) detector, water content was determined by a Karl-Fisher coulometer, and total residual solvents and nonvolatiles/inorganics were checked simultaneously by thermogravimetric analysis (TGA). The purity of the $17{\beta}$-estradiol was 985.6 mg/g and the expanded uncertainty was 2.1 mg/g at 95% confidence. The developed method can be applied to the development of certified reference materials, which play a critical role in traceability.

• Preventive Nutrition and Food Science
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• v.18 no.2
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• pp.145-149
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• 2013

We tested for residual pesticide levels in dried vegetables in Seoul, Korea. A total of 100 samples of 13 different types of agricultural products were analyzed by a gas chromatography-nitrogen phosphate detector (GC-NPD), an electron capture detector (GC-${\mu}ECD$), a mass spectrometry detector (GC-MSD), and a high performance liquid chromatography- ultraviolet detector (HPLC-UV). We used multi-analysis methods to analyze for 253 different pesticide types. Among the selected agricultural products, residual pesticides were detected in 11 samples, of which 2 samples (2.0%) exceeded the Korea Maximum Residue limits (MRLs). We detected pesticide residue in 6 of 9 analyzed dried pepper leaves and 1 sample exceeded the Korea MRLs. Data obtained were then used for estimating the potential health risks associated with the exposures to these pesticides. The estimated daily intakes (EDIs) range from 0.1% of the acceptable daily intake (ADI) for bifenthrin to 8.4% of the ADI for cadusafos. The most critical commodity is cadusafos in chwinamul, contributing 8.4% to the hazard index (HI). This results show that the detected pesticides could not be considered a serious public health problem. Nevertheless, an investigation into continuous monitoring is recommended.

• YAKHAK HOEJI
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• v.55 no.1
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• pp.64-68
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• 2011

In this study, a high performance liquid chromatography-diode array detector method was established, for simultaneous determination of three compounds, berberine, palmatine and geniposide in Hwangryunhaedok-tang, To develop and validate method, $C_{18}$ column (5 ${\mu}M$, 4.6 mm${\times}$250 mm) was used with gradient mobile phase, water containing 0.1% trifluoroacetic acid (TFA) and MeOH at the column temperature of $30^{\circ}C$. UV wavelength was set at 230 and 280 nm. Validation of the chromatography method was evaluated by linearity, precision and accuracy test. Calibration curve of standard components showed good linearity ($R^2$ > 0.9999). The limits of detection (LOD) and limits of quantification (LOQ) varied from 0.05 to 0.17 ${\mu}g/ml$ and 0.15 to 0.53 ${\mu}g/ml$, respectively. The relative standard deviations (RSDs) data of intra-day and inter-day test were in less than 2.99% and 1.90%, respectively. The results of the accuracy test were in the range of 98.36 to 102.52% with RSDs values 0.32 to 1.98%. The results of validation indicated that this method was a very accurate and sensitive assay.

• The Korea Journal of Herbology
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• v.27 no.6
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• pp.43-48
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• 2012

Objectives : This study was investigated to determine the contents of pesticide residues and sulfur dioxide residues in commercial herbal medicines in Korea. Methods : Chromatographic test was performed on 100 samples consisted with 10 kinds of medicinal plants including improted and domestic products. To establish 19 pesticide residues (DDE, DDD, DDT, Dieldrin, Methoxychlor, BHC isomers, Aldrin, Endosulfan isomers, Endrin, Captan, Procymidone, Chlorpyrifos and Imidacloprid) in commercial herbal medicines, chromatographic equipments were used with the gas chromatography-mass detector and gas chromatography-electron capture detector for qualitative analysis. The imidacloprid analysis was performed by high performance liquid chromatograpgy-ultraviolet detector at 270 nm UV wavelength. The contents of sulfur dioxides were analyzed by modified Monnier-Williams method. All methods were based on notification procedure of Korea Food & Drug Administration (KFDA). Results : The residual pesticides were not founded in improted and domestic samples. Among 100 samples, the residues of sulfur dioxide in 73 samples were not detected and 25 samples showed contents in the range of 0~21.90 mg/kg. The excess samples of MRLs were 2 samples (30 mg/kg to medicinal herbs), Asiasari Radix et Rhizoma (Imported product) and the average amount of sulfur dioxide in 2 unsuitable samples were 14.83 mg/kg. These samples were found to transgress KFDA regulatory guidance of residual sulfur dioxide. Conclusion : These results are able to use as basic data to improve the reliability and value of commercial medicinal herbs.

• Korean journal of food and cookery science
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• v.18 no.2
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• pp.173-178
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• 2002

Fresh Shiitake mushrooms were irradiated by UV-B or dried by using hot air to increase the vitamin D$_2$content. Vitamin D$_2$content was determined by high-performance liquid chromatography Irradiating the inside of the mushroom cap was more effective in increasing vitamin D$_2$content than irradiating the outside of the mushroom cap. Irradiation of UV-B at 0, 2.5, 5.0, 7.5 and 10 J/㎠ increased the content of vitamin D$_2$in the mushroom to 21.51, 120.78, 144.38, 168.08, and 187.69 $\mu\textrm{g}$/g, respectively. Vitamin D$_2$content of Shiitake mushrooms with irradiation of 10 J/㎠ decreased from 187.69 to 98.78 $\mu\textrm{g}$/g by 6 hours of hot-air drying. When three kinds of drying method (UV-B irradiation followed by hot-air drying, hot-air drying, and sunlight drying) were compared, the combination of UV-B irradiation and hot-air drying was the most effective in terms of increasine the vitamin D$_2$content in the mushroom.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.23 no.3
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• pp.101-107
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• 1997

Phellinus linteus was artificially cultivated in kangwon province in Korea. The air-dried phellinus linteus was frozen in liquid nitrogen tank and powdered in jar. 10g of the powder was extracted with each 200g of ethanol, methanol, distilled water and 1,3-butylene glycol/distilled water 4 hours under refluxing and then the liquidextract was concentrated under reduced pressure. As a result of analysis by high performance liquid chromatography and thin layer chromarography, many kinds of sugar and flavonoids were detected. Also we knew that phellinus linteus' extract had a strong UV-ray absorption. In the efficacy test for applying to cosmetics, free radical scavenging effect was confirmed. As a result, 2% of sample was the most potent inhibitory effect and the free radical savenging activity, was 0.31%. This is more effective than any other meterial. In the test of antioxidative activity against lipid autoxidation, phellinus linteus' extract had a good effect by 46% while vitamine E was 42.3%. The immunological activity of phellinus linteus was showed through the activation of macrophage cell. Actually, phellinus linteus activated macrophage function of 1.1-1.8 times including nitrite production compared to control. The whitening effect of phellinus linteus was showed through the inhibition of tyrosinase activity, melanin biosynthesis of S. bikiniensis and B-16 melanoma cells. Phellinus linteus' extract was showed strong mushroom tyrosinase inhibitory activity with IC50 value of 0.5% and inhibited melanin biosynthesis with 28mm inhibition zone at 0.005%/paper disc in S. bikinniensis, a bacterium used as an indicator organism in this work. Also it inhibited melanin biosynthesis in B-16 melanoma cells with a minimum inhibitory concentration of 0.134%.

• Journal of Food Hygiene and Safety
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• v.26 no.1
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• pp.16-24
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• 2011

A method was established for the simultaneous determination of sugar alcohols, erythritol, xylitol, sorbitol, inositol, mannitol, maltitiol, lactitol and isomalt by High Performance Liquid Chromatography (HPLC). The sugar alcohols were converted into strong ultraviolet (UV)-absorbing derivatives with p-nitrobenzoyl chloride (PNBC). HPLC was performed on Imtakt Unison US-$C_18$ column, using acetonitrile: water (77:23) as a mobile phase and UV detection (260 nm). The calibration curves for all sugar alcohols tested were linear in the 10~200 mg/L range. The average recoveries of the sugar alcohols from three confectioneries spiked at 100 ppm of eight sugar alcohol standards ranged from 81.2 to 123.1% with relative standard deviations ranging fromo 0.2 to 4.9%. The limits of detection (LODs) were $0.5{\sim}8\;{\mu}g/L$ and the limits of quantification (LOQs) were $2{\sim}17\;{\mu}g/L$. Reproducibility of 8 sugar alcohols was 0.28~1.97 %RSD. The results of the analysis of confectioneries showed that 89 samples of 130 were detected and the sugar alcohols content of samples investigated varied between 0.4 and 693.7 g/kg. A method for the simultaneous determination of eight sugar alcohols will be used as basic data for control of sugar alcohols in confectioneries, and quality control in food manufacturing.

• Journal of Food Hygiene and Safety
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• v.38 no.5
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• pp.297-304
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• 2023

Domoic acid (DA), a neurotoxin produced naturally by diatoms, is responsible for incidents of amnesic shellfish poisoning. In this study, a modified analytical method was established to determine domoic acid in seafood using solid phase extraction cleanup and optimizing the amount of sample and extraction solvent to reduce interference effects. The modified method using high-performance liquid chromatography with ultraviolet detection was validated using three seafood matrices (mussel, red snow crab, and anchovy) at three concentrations (1, 2, and 4 mg/kg) and compared to the Food Code method. Compared to the Food Code method, the modified method showed better performance in terms of linearity (R²>0.999), detection limit (0.02-0.03 mg/kg), quantification limit (0.05-0.09 mg/kg), intra-/inter-day accuracy (86.2-100.4%), and intra-/inter-day precision (0.2-4.0%). Furthermore, the method was successfully applied for the analysis of 87 seafood samples marketed in Korea, and DA was detected at a low concentration of 140 ㎍/kg in one anchovy sample. These results suggest that the modified method can be used for routine determination of DA in seafood.