• Journal of Pharmacopuncture
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• v.18 no.1
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• pp.44-55
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• 2015

Objectives: Scolopendra subspinipes mutilans (S. subspinipes mutilans) is known as a traditional medicine and includes various amino acids, peptides and proteins. The amino acids in the pharmacopuncture extracted from S. subspinipes mutilans by using derivatization methods were analyzed quantitatively and qualitatively by using high performance liquid chromatography (HPLC) over a 12 month period to confirm its stability. Methods: Amino acids of pharmacopuncture extracted from S. subspinipes mutilans were derived by using O-phthaldialdehyde (OPA) & 9-fluorenyl methoxy carbonyl chloride (FMOC) reagent and were analyzed using HPLC. The amino acids were detected by using a diode array detector (DAD) and a fluorescence detector (FLD) to compare a mixed amino acid standard (STD) to the pharmacopuncture from centipedes. The stability tests on the pharmacopuncture from centipedes were done using HPLC for three conditions: a room temperature test chamber, an acceleration test chamber, and a cold test chamber. Results: The pharmacopuncture from centipedes was prepared by using the method of the Korean Pharmacopuncture Institute (KPI) and through quantitative analyses was shown to contain 9 amino acids of the 16 amino acids in the mixed amino acid STD. The amounts of the amino acids in the pharmacopuncture from centipedes were 34.37 ppm of aspartate, 123.72 ppm of arginine, 170.63 ppm of alanine, 59.55 ppm of leucine and 57 ppm of lysine. The relative standard deviation (RSD %) results for the pharmacopuncture from centipedes had a maximum value of 14.95% and minimum value of 1.795% on the room temperature test chamber, the acceleration test chamber and the cold test chamber stability tests. Conclusion: Stability tests on and quantitative and qualitative analyses of the amino acids in the pharmacopuncture extracted from centipedes by using derivatization methods were performed by using HPLC. Through research, we hope to determine the relationship between time and the concentrations of the amino acids in the pharmacopuncture extracted from centipedes.

• Journal of Korean Society of Environmental Engineers
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• v.32 no.6
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• pp.639-648
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• 2010

The optimal conditions for the analysis of BPA by HPLC-MS/MS was investigated and the ultrasound degradation capacity of the BPA, with the goal to establish the proper directions for analyzing infinitesimal quantities of BPA by HPLC-MS/MS was examined. The MDL and LOQ of BPA analyzed by HPLC-MS/MS were measured 0.13 nM and 1.3 nM respectively, its sensitivity about 620 and 32 times greater than HPLC-UV (MDL: 81.1 nM, LOQ: 811 nM) and FLD (MDL: 4.6 nM, LOQ: 46 nM). In other words, the new method enables the analysis of BPA with the accuracy up to one 1,180th of the amount specified in U.S. EPA guideline for drinking water. Degradation rate of BPA by ultrasound measured over 95% under 580 kHz and 1000 kHz frequency within 30 minutes of treatment, whereas the rate showed some decrease at 28 kHz frequency. At 580 kHz of ultrasound has proven to be the most effective among others at degradation rate and $k_1$ value, so we concluded that this frequency of ultrasound creates hospitable condition for the combined process of degradation by pyrolysis and oxidization. With the addition of 0.01 mM of $CCl_4$, BPA with the initial concentration of 1 ${\mu}M$ was degraded by more than 98% within 30 minutes, the $k_1$ value measured 5 minutes and 30 minutes into the experiment both showed increases by 1.4 and 1.1 times, respectively, compared with BPA without $CCl_4$. It is also found that the main degradation mechanism of BPA by ultrasound is oxidization process by OH radical, based on the fact that the addition of 10 mM of t-BuOH decreased the rate of BPA degradation by around 60%. However, 33% of BPA degradation rate obtained with the addition of t-BuOH implies further degradation done by pyrolysis or other sorts of radical beside OH radical.

• Korean Journal of Food Science and Technology
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• v.46 no.3
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• pp.276-282
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• 2014

An accurate and sensitive analytical method was established for the simultaneous determination of synephrine and n-methyltyramine contents by ultra-performance liquid chromatography (UPLC) with a fluorescence detector (FLD). A 70:30 (v/v) mixture of 10 mM sodium dodecyl sulfate (SDS) and acetonitrile was used as the mobile phase. The coefficient of correlation ($r^2$) was 0.9999 for both synephrine and n-methyltyramine, and their limits of detection (LOD) were 0.02 and 0.01 mg/kg, respectively. The percentage recoveries for synephrine and n-methyltyramine were 96.4% and 100.9%, respectively, from bitter orange (Citrus aurantium) samples. The synephrine and n-methyltyramine contents were 38.07-118.21 mg/kg and 0.27-0.56 mg/kg, respectively, in the orange fruit samples, while they were 14.61-120.39 mg/kg and up to 3.34 mg/kg, respectively, in the tested commercial orange juice samples. The differences in synephrine and n-methyltyramine content between orange fruit and commercial orange juice were not significant (p<0.05). These results suggest that UPLC-FLD can be applied to develop an analytical method of quality control for commercial orange juice.

• Journal of Food Hygiene and Safety
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• v.26 no.3
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• pp.214-221
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• 2011

Deoxynivalenol (DON) and zearalenone (ZEN) are mainly contaminated mycotoxins in feeds. The study was carried out to analyze and survey the contamination of DON and ZEN in one hundred thirteen samples of feeds. After cleaning all samples with immunoaffinity column, the mycotoxins were analysed by using high performance liquid chromatography/fluorescence with diode array detector (HPLC/FLD with DAD). The average recoveries of DON were 88.76 and 95.40% at the levels of 200 and 1,000 ${\mu}g/kg$ and 87.09 and 98.40% of ZEN were recovered at the levels of 100 and 500 ${\mu}g/kg$, respectively. The limit of detection (LOD) were 6.0 and 3.0 ${\mu}g/kg$ for DON and ZEN, respectively. The average concentrations of DON were 372.1, 324.0 and 990.9 ${\mu}g/kg$ in chicken, pig and cattle feed, respectively. Those of ZEN were 76.1, 43.7 and 196.2 ${\mu}g/kg$ for them, individually.

• Korean Chemical Engineering Research
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• v.56 no.6
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• pp.832-840
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• 2018

In this study, both of the concentration of benzo(a)pyrene in 5 species (total 50 samples) of medicinal herbs and their transfer ratios in the preparation steps of water extract(decoction) and soft extract, were measured by HPLC/FLD. The calibration curve of benzo(a)pyrene shows excellent correlation over the concentration range of 3~40 ng/mL with the correlation coefficient ($R^2$) of 1.000. The detected benzo(a)pyrene concentrations from the medicinal herbs ranged from non-detection to $37.54{\mu}g/kg$, and their average was $6.73{\mu}g/kg$. Among the total samples, 15 samples (i.e., 30%) exceeded the limit of herbal medicine benzo(a)pyrene criteria (i.e., $5{\mu}g/kg$) according to the notification No. 2009-302 from Ministry of Food and Drug Safety. In particular, the concentration of benzo(a)pyrene in Coptidis Rhizome was turned out to be the highest of $37.54{\mu}g/kg$. The detected benzo(a)pyrene concentrations from water extract(decoction), soft extract and remnant after boiling, ranged from non-detection to $2.31{\mu}g/kg$, non-detection to $2.28{\mu}g/kg$, and 2.18 to $21.91{\mu}g/kg$, respectively. In preparation of water extract(decoction) and soft extract, transferred benzo(a)pyrene was not detected or, if transferred, the maximal transfer ratios of benzo(a)pyrene were shown to be 8.9% and 9.8%, respectively. Therefore, the content of benzo(a)pyrene in the samples of herbal medicine used in this study, were reduced by more than 90% in preparation steps of water extract (decoction) and soft extract.

• Journal of Radiation Industry
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• v.6 no.3
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• pp.205-209
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• 2012

The decomposition of 50 pesticides present in an aqueous solution using ${\gamma}-irradiation$ from a $^{60}Co$ gamma-ray source was investigated using laboratory-scale experiment. The rates of decomposition were determined using a gas chromatography-electron capture detector (GC-ECD), high-performance liquid chromatography-photo diode array detector (HPLC-PDA), and HPLC-fluorescence detector (FLD). When the initial concentration of pesticides was 10 ppm, and the radiation dose was 2, 5, 10, 20, and 30 kGy, respectively, 14 pesticide samples showed high removal rates (>50%) at absorbed doses of more than 10 kGy. With the exception of procymidone, they were all completely removed at a 30 kGy irradiation dose. These results provide fundamental data on the reactivity between gamma-irradiation and pesticides in an aqueous solution. Further, an evaluation of the toxicity of radiolytic intermediate products is required.

• Food Science of Animal Resources
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• v.41 no.4
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• pp.731-738
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• 2021

Herein, a novel analytical method using a high-performance liquid chromatography-fluorescence detector (HPLC/FLD) is developed for rapidly measuring an L-carnitine ester derivative in infant powdered milk. In this study, solid-phase extraction cartridges filled with derivatized methanol and distilled water were used to effectively separate L-carnitine. Protein precipitation pretreatment was carried out to remove the protein and recover the analyte extract with a high recovery (97.16%-106.56%), following which carnitine in the formula was derivatized to its ester form. Precolumn derivation with 1-aminoanthracene (1AA) was carried out in a phosphate buffer using 1-(3-dimethylaminopropyl)-3-ethylcarbodiimide hydrochloride (EDC) as the catalyst. Method validation was performed following the AOAC guidelines. The calibration curves were linear in the L-carnitine concentration range of 0.1-2.5 mg/L. The lower limit of quantitation and limit of detection of L-carnitine were 0.076 and 0.024 mg/L, respectively. The intra- and interday precision and recovery results were within the allowable limits. The results showed that our method helped reduce the sample preparation time. It also afforded higher resolution and better reproducibility than those obtained by traditional methods. Our method is suitable for detecting the quantity of L-carnitine in infant powdered milk containing a large amount of protein or starch.

• The Korean Journal of Food And Nutrition
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• v.32 no.1
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• pp.61-68
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• 2019

In this study, the contents of water-soluble vitamins $B_1$ (thiamin), $B_2$ (riboflavin), $B_3$ (niacin), and $B_{12}$ (cyanocobalamin) in namuls (wild greens), such as salads and side dishes, consumed in Korea were quantified by high-performance liquid chromatography (HPLC) with UV and fluorescence detection. All samples were prepared with recipes used in Korea. All analyses were performed under the quality control of vitamin $B_1$, $B_2$, $B_3$, and $B_{12}$. The vitamin $B_1$, $B_2$, and $B_3$ contents in namuls consumed in Korea were analyzed. The highest content of vitamin $B_1$ was $3.018{\pm}0.016mg/100g$ in Putgochudoenjang-muchim. The highest contents of vitamin $B_2$, $B_3$, and $B_{12}$ were $0.279{\pm}0.003mg/100g$ in Gul-muchim, $12.241{\pm}0.040mg/100g$ in Chamchi-salad, and $8.133{\pm}0.371{\mu}g/100g$ in Pijogae-muchim, respectively. These results showed that animal-based ingredients in salads provided for good intake of vitamin $B_{12}$. These results can be used as basic data for food composition tables and improvement of the national health of Koreans.

• Journal of Food Hygiene and Safety
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• v.32 no.3
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• pp.187-192
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• 2017

The consumption of herbal medicines has been increasing with growing interest in health. However, due to recent climate change and the complex distribution process of herbal medicines with high import dependence the likelihood of contamination with mycotoxin has been increased. Mycotoxins are emerging as key indicators for ensuring safety of herbal medicines. A total of 498 herbal medicine samples were screened for mycotoxin contamination in this study. Aflatoxin in the herbal medicine samples was extracted by using immunoaffinity column, then the extracted aflatoxin was quantified via high performance liquid chromatography coupled with fluorescence detection (HPLC-FLD) method. The extraction method was verified by linearity, recovery, LOD and LOQ. Aflatoxins were detected in 39/498 samples in an average of $7.670{\mu}g/kg$ ($0.610-77.452{\mu}g/kg$ range). Although safety standards for Corydalis Tuber is not currently available in korea, five of the 39 samples had high concentration of aflatoxins (average of $14.9{\pm}4.1{\mu}g/kg$). In conclusion, it is urgent to establish safety criteria of aflatoxin in Corydalis Tuber. The results of the current study suggest that continuous monitoring is necessary for proactive management of herbal medicine safety.

• The Korean Journal of Pesticide Science
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• v.16 no.1
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• pp.43-53
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• 2012

In order to monitor the levels of pesticides in environment-friendly stalk and stem vegetables and leafy vegetables selling at markets in Korea. A total of 637 (395 organic agricultural products, 242 pesticide-free agricultural products) samples of 21 stalk and stem vegetables and leafy vegetables were collected twice from markets in July and August 2010 in Korea. Pesticide residues in samples were analyzed by multiresidue method for 240 pesticides using GC-ECD/NPD and HPLC-DAD/FLD. The suspected-pesticides were confirmed with a GC-MSD. As a result of analysis, six pesticides were detected from eight samples, representing a detection rate of 1.3% and amounts of pesticide residues in samples were as follows: alachlor 0.043, chlorfenapyr 0.022-0.324, diazinon 0.024, dicofol 0.009-0.138, dithiopyr 0.008, metolachlor 0.025 mg/kg. Their residue levels were below the MRLs. Estimated daily intakes (EDIs) of the pesticides detected from stalk and stem vegetables and leafy vegetables were less than 25% of their acceptable daily intakes (ADIs), representing that residue levels of the pesticides detected were evaluated as safe for consumption. However, five samples containing pesticide residues were unsuitable environment-friendly products because of pesticides detected more than their 10% MRLs in organic and pesticide-free agricultural products.