• Korean Journal of Food Science and Technology
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• v.52 no.1
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• pp.26-30
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• 2020

This study was undertaken to determine the characteristics of xanthoangelol, the major chalcone constituent derived from the extracts of different parts of Lespedeza bicolor. Xanthoangelol was isolated from the root extract using column chromatography and used as a standard for quantitative analysis. The structure of the isolated compound was established based on spectroscopic evidence. The HPLC-DAD method was validated for specificity, linearity, precision, accuracy, limit of detection, and limit of quantitation. The calibration curve of xanthoangelol had significant linearity (R²>0.9999). Limit of detection and limit of quantitation 0.018 and 0.059 ㎍/mL, respectively. The relative standard deviation values of precision test, and intra- and inter-day tests were less than 0.22 and 0.40%, respectively. In the recovery test, the accuracy ranged from 98.98-102.78% with RSD values less than 0.13%. The method validation parameters indicate the applicability of the HPLC method for quality control of food or drug formulations containing L. bicolor.

• Journal of Environmental Health Sciences
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• v.42 no.1
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• pp.53-60
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• 2016

Objectives: Preservatives are commonly used in pharmaceuticals, cosmetics and other products to extend the expiration date and prevent the growth of microorganisms. Preservatives are generally effective in controlling mold and inhibiting yeast growth, and against a wide range of bacterial attacks as well. They also adversely affect the quality of sperm and cause precocious puberty in children. This study was performed to analyze seven preservatives used in pharmaceuticals and personal care products. Methods: Five kinds of pharmaceuticals and personal care products (PPCPs) were examined for analysis with a high performance liquid chromatography-diode array detector. Each sample was homogenized and the targeted compounds were extracted with methanol. The suspended particulate was removed by syringe filter. Next, the sample was injected into an HPLC system. The separation of the seven preservatives was achieved with a C18 column and gradient mode. The accuracies were between 73% and 120% and precision was lower than 11.58% (RSD). Results: All of the calibration curves showed good linearity with a coefficient of determination ($r^2$) over 0.999. Among the PPCP samples, the detection rate of preservatives was 32.5% for pharmaceuticals, 44.8% for toothpaste, 76.9% for mouthwash, 40.0% for body lotion and 56.0% for wet tissues. The average concentrations of the preservatives in PPCPs were BA 1141.0 mg/kg, MP 709.8 mg/kg, EP 624.9 mg/kg, PP 216.9 mg/kg, BP 167.8 mg/kg, and TCS 538.2 mg/kg. The most frequently detected preservatives in pharmaceuticals and personal care products were BA, MP and PP. The concentrations of preservatives exceeded Korean regulatory standards in 11 samples of medicines, three of mouthwash and two of body lotion. Conclusion: We found that most of the PPCP samples contained various preservatives. It is necessary to identify which preservatives were used and to determine the level of preservatives in PPCPs and to assess the health risk to susceptible populations such as children.

• Journal of the Korean Society of Food Science and Nutrition
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• v.31 no.4
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• pp.604-608
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• 2002

Accelerated solvent extraction (ASE) was used for a rapid and simple extraction of propylenchlorohydrin (PCH) residue in hydroxylpropyl modified starch. The effects of temperature, pressure and extraction solvent on the extraction efficiency were investigated to find the optimal condition of ASE. The optimal conditions for PCH extraction in hydroxylpropyl modified starch were static time of 50 min, purge time of 300 sec, heating time of 5min, temperature of 12$0^{\circ}C$, pressure of 2500 psi, flush (%) with 100 volumes, and ethylacetate as an extraction solvent. The recovery (96.1%) of this method was higher than that (76.4%) of Code of Food Additive. Therefore, the ASE was a good method in both aspects of efficiency and effectiveness.

• The Korea Journal of Herbology
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• v.26 no.1
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• pp.41-46
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• 2011

Objectives : To quantitate the main compounds and investigate the biological activity of Sosiho-tang (Xiao-Chai-Hu-Tang, SST), simultaneous determination of baicalin and glycyrrhizin, and anti-inflammatory activity were estimated. Methods : A quantitative analysis was performed using a high performance liquid chromatography (HPLC). Reference compounds were separated on a reversed-phase column using gradient elution with water and acetonitrile each containing acetic acid at a flow rate of 1 mL/min. And the productions of nitric oxide (NO) and prostaglandin $(PE)E_2$ were examined by lipopolysaccharide (LPS)-treated RAW 264.7 cells in the presence of the SST. The anti-inflammatory activity of SST was investigated by carrageenin-induced paw edema in rats. The paw volume was measured at 2 and 4 hr following carrageenin-induced paw edema in rats. Results : The correlation coefficients of the compounds showed good linearity ($r^2$ > 0.9992) over the linear range. The precisions of intra- and inter-day were less than 7.0% of relative standard deviation (RSD) values for baicalin and less than 3.5% of RDS valuse for glycyrrhizin. Recovery rates were within the range of 95.41-101.5%. The contents of baicalin and glycyrrhizin in SST were average 70.52, 6.18 mg/g, respectively. And SST exhibited inhibitory effect on NO production in LPS-treated RAW 264.7 cells but not on $PGE_2$ production. Oral administration of SST (1 g/kg) showed a reduction in carrageenin-induced paw edema on rats. Conclusions : The analytical method was applied successfully to measure the contents of baicalin and glycyrrhizin in SST which exhibited anti-inflammatory activities.

• Journal of the Korean Society of Food Science and Nutrition
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• v.32 no.7
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• pp.965-970
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• 2003

This study has been performed to develope a method for the simultaneous determination of 1,4-dioxane (DOX), epichlorohydrin (EPC), propylene chlorohydrin (PCH), ethylene chlorohydrin (ECH) and 1,3-dichloro-2-pro-panol (DCP) in polysorbates, chloline chloride, choline bitartrate, modified starch and spices by purge and trapgas chromatography. Experimental design was used to select a suitable trap by measuring the limit of detection (LOD) and to investigate the effect of temperature and salt of extraction, and the percentage of recovery in various matrix. The LOD of DOX, EPC, PCH, ECH and DCP were 1.38$\mu\textrm{g}$, 0.23$\mu\textrm{g}$, 3.30$\mu\textrm{g}$, 3.97$\mu\textrm{g}$, 20.43$\mu\textrm{g}$ respectively, by means of using Vorcarb 3000 trap with 5$0^{\circ}C$ sample sparger. Excluding EPC, the recoveries of target compounds were above 90% in all matrix. Target compounds in polysorbates (17), choline chloride (5), choline bitartrate (5), modified starch (8) and spices (25) were not detected. But 2.5 ppm of DOX was detected in Tween 80.

• Korean Journal of Environmental Agriculture
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• v.35 no.1
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• pp.6-14
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• 2016

BACKGROUND: Residual organochlorine pesticides (OCPs) are chemical substances that persist in the environment, bioaccumulate through the food web, and pose a risk of causing adverse effect to human health and the environment. They were designated as persistent organic pollutants (POPs) by Stockholm Convention. Greenhouse strawberry is economic crop in agriculture, and its cultivation area and yield has been increased. Therefore, we tried to investigate the POPs residue in greenhouse soil and strawberry.METHODS AND RESULTS: Extraction and clean-up method for the quantitative analysis of OCPs was developed and validated by gas chromatography (GC) with electron capture detector (ECD). The clean-up method was established using the modified quick, easy, cheap, effective, rugged, and safe(QuEChERS) method for OCPs in soil and strawberry. Limit of quantitation (LOQ) and recovery rates of OCPs in greenhouse soil and strawberry were 0.9-6.0 and 0.6-0.9 μg/kg, 74.4-115.6 and 75.6-88.4%, respectively. The precision was reliable sincerelative standard deviation (RSD) percentage (0.5-3.7 and 2.9-5.2%) was below 20, which was the normal percent value. The residue of OCPs in greenhouse soil was analyzed by the developed method, and dieldrin, β-endosulfan and endosulfan sulfate were detected at 1.6-23, 2.2-28.4 and 1.8-118.6 μg/kg, respectively. Those in strawberry were not detected in all samples.CONCLUSION: Dieldrin, β-endosulfan and endosulfan sulfate in a part of investigated greenhouse soil were detected. But those were not detected in investigated greenhouse strawberry. These results showed that the residue in greenhouse soil were lower level than bioaccumulation occurring.

• Analytical Science and Technology
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• v.25 no.1
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• pp.25-32
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• 2012

Isotope dilution mass spectrometry (ID-MS) based on liquid chromatography tandem mass spectrometry (LC/MS/MS) was developed for the accurate determination of sorbic acid in tea-drink. An isotope analogue of sorbic acid, $^{13}C_2$-sorbic acid, was obtained by custom synthesis. MS was operated in the negative mode with selected reaction monitoring (SRM) mode of $[M-H]^-$ ${\rightarrow}$ $[M-CO_2H]^-$ channel at m/z 111 ${\rightarrow}$ 67 for sorbic acid and at m/z 113 ${\rightarrow}$ 68 for its isotope analogue. Chromatographic separation was accomplished with a C18 column and an isocratic mobile phase of 55% of 50 mM ammonium acetate (pH 4.5) and 45% of methanol. Homogeneous reference materials were prepared for validation of this method, including repeatability and reproducibility tests, by fortifying tea-drink with sorbic acid in our laboratory. Repeatability and reproducibility studies showed that the ID-LC/MS method is a reliable and reproducible method which provides less than 3.8% of relative standard deviation (RSD) for the analysis of sorbic acid.

• Journal of Physiology & Pathology in Korean Medicine
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• v.30 no.2
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• pp.88-94
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• 2016

The study was carried out to examine the anti-obesity effects of 40% ethanol extract from green tea seed (GS) and quantitative determination of caffeine as its major compound. The specificity was satisfied with retention time and UV spectrum by analysis of caffeine using HPLC and comparison with standard compound. It showed a high linearity in the calibration curve with a coefficient of correlation (R²) of 0.9974. The amount of caffeine in GS was about 4.649 mg/g (0.465%) in the three times analysis, and relative standard deviation (RSD) was less than 0.452% by the validated method. The anti-obesity effects of GS were evaluated by using Oil Red O staining in 3T3-L1 adipocytes and body weight, visceral fat and lipid profiles in high fat diet (HFD)-induced C57BL/6 obese mice. Our results indicated that treatment with GS dose-dependently decreased lipid accumulation contents (p<0.001). Moreover, after oral administration for 30 days feeding with HFD-induced obses mice, GS (100 and 300 mg/kg/day) produced a significant decrease in serum total cholesterol (TC), glutamic oxaloacetic transaminase (GOT), glutamic pyruvic transaminase (GPT) and visceral fat. Thus, the result of this study indicate that the GS may be a useful resource for the management of obesity.

• Korean Journal of Food Science and Technology
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• v.40 no.3
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• pp.354-359
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• 2008

A survey for zearalenone contamination was conducted on 27 soy bean samples, 27 red bean samples, 16 black bean samples, 19 seoritae samples, 14 seomoktae samples, for a total of 127 commercial Korean samples. Zearalenone was quantified by the immunoaffinity column clean-up method with high performance liquid chromatography-fluorescence detection (HPLC-FLD), and was confirmed by liquid chromatography tandem mass spectrometry(LC-MS/MS). The limits of detection and quantification were $2.0{\mu}g/kg$ and $6.0{\mu}g/kg$, respectively. The recovery in the beans ranged from 82.2 to 98.4%. According to HPLC-FLD, zearalenone was detected in 13 samples (10.2% incidence), including 1 soybean and 12 red bean samples. The zearalenone contamination levels were in the range of 8.01${\sim}38.98{\mu}g/kg$. Finally, LC-MS/MS analysis was conducted in the contaminated samples to verify the results of HPLC-FLD. The LC-MS/MS results confirmed the presence of zearalenone in all 13 samples. The contamination level was lower than that of EU, which is below $100{\mu}g/kg$ for raw grains.

• Analytical Science and Technology
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• v.16 no.6
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• pp.483-487
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• 2003

Amitrole is well-known as a non-selective herbicide and it is able to cause contamination of driking water as well as pollution of ground water and surface water. However, it is difficult to extract from water because it has a high solubility for water whereas a low solubility for general organic solvents. This method is described for the determination of amitrole in water samples by GC/MS. After evaporation of 10 mL water sample by a vacuum evaporator, amitrole was derivatized with isobutyl chloroformate (iso-BCF) on room temperature for 15~20 min. As a result, the sensitivity for GCfMS was improved as N-isobutoxycarbonyl amitrole derivative was formed. The linearity of the calibration curve showed good as 0.997. The recoveries were obtained more than 94.9% and relative standard deviations were less than 2.8% at $1.0{\mu}g/L$, $10.0{\mu}g/L$ and $100.0{\mu}g/L$. The limit of detection showed $0.1{\mu}g/L$ with a signal-to-noise ratio (S/N) of 3.