• 한국식품위생안전성학회지
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• 제26권3호
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• pp.214-221
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• 2011

2010년 유통사료 113점에 대하여 곰팡이독소 오염도 조사를 실시하였다. 면역친화컬럼(IAC)을 이용하여 각각 정제하였으며, HPLC/DAD와 FLD를 연결하여 동시분석하였다. DON은 200과 1,000 ${\mu}g/kg$수준에서 각각 95.40과 88.76%의 회수율과 4.03과 1.40%의 상대표준편차(%RSD)를 나타내었다. ZEN은 100과 500 ${\mu}g/kg$ 수준에서 각각 87.09과 98.40%의 회수율과 9.01과 2.81%의 상대표준편차(%RSD)를 나타내었다. 배합사료인 닭사료, 돼지사료, 소사료에서 DON과 ZEN이 각각 372.1, 324.0, 990.9 ${\mu}g/kg$와 76.1, 43.7, 196.2 ${\mu}g/kg$의 평균오염도를 보여 2009년도 조사결과보다 높은 오염수준을 나타내었다. 옥수수, 단백피, 주정박, 옥수수배아박, 옥수수글루텐에서는 DON과 ZEN이 각각 224.6, 3150.4, 721.5, 37.8, 207.3 ${\mu}g/kg$와 77.8, 308.5, 163.1, 116.9, 510.8 ${\mu}g/kg$로 나타남에 따라 역시 배합사료에 곰팡이독소를 오염시키는 주 원인물질로 확인되었다.

• 한국식품위생안전성학회지
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• 제31권5호
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• pp.311-318
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• 2016

국내 미지정 색소인 azorubine에 대한 우리나라의 공인분석법을 설립하기 위해 제외국의 공인분석법들(유럽연합의 EFSA, 영국의 FSA, 우리나라의 식품의약품안전평가원)이 비교되었다. 재현된 HPLC 방법들 중 FSA의 분석법이 가장 우수한 분석 결과를 나타내어 azorubine분석법으로 최종 선정되었다. Azorubine 분석을 위한 위 세 기관의 전처리 방법은 모두 낮은 회수율을 나타내었다. 따라서 식품의약품안전평가원의 전처리법을 개선한 새로운 전처리 방법이 개발되었다. 최종 선정된 HPLC 분석법과 본 연구를 통해 개발된 새로운 식품 전처리법에 대한 분석법 밸리데이션을 실시하였다. 검증 실험에서 음료류에서 97~103%, 빵 및 과자류에서 95~101%, 기타 식품에서 93~102%의 회수율을 나타내었고, 실험실간 교차검증에서 -1.29~0.26의 z-score를 보여 신뢰할 수 있는 것으로 판단되었다. 이 결과로부터 본 연구에서 확립된 전처리법 및 분석법은 미지정 색소 azorubine이 사용된 식품검사에 활용될 수 있는 분석법으로 확인되었다.

• 생약학회지
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• 제45권4호
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• pp.338-345
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• 2014

HPL-4 is a new herbal formulation developed for the treatment of osteoarthritis. In this study, we took HPL-4 to develop a method for simultaneous determination of nine marker compounds (protocatechuic acid, chlorogenic acid, liriodendrin, nodakenin, ${\beta}$-$\small{D}$-(3-O-sinapoyl)frucofuranosyl-${\alpha}$-$\small{D}$-(6-O-sinapoyl)glucopyranoside, quercitrin, 6-gingerol, decursin and decursinol angelate) present in the formulation. The analytes were separated by UPLC system consisting of diode array detector at 205 nm and RP-amide column, and solvent system of $ACN/0.1%H_3PO_4$. Analytical method was validated to evaluate its linearity, limit of detection (LOD), limit of quantification (LOQ), precision, and accuracy. All standards showed good linearity ($R^2$ >0.99) in the rage of $0.25-400.0{\mu}g/mL$. The LOD and LOQ were within the range of 0.021-0.148 and $0.070-0.448{\mu}g/mL$, respectively. Intra- and inter-day precision was less than RSD 4.0% and the accuracy was range from 92.00-104.81% with RSD<4.2%. The results suggest that the developed UPLC method is precise, accurate and effective, and could be applied for quality control of HPL-4 formulation.

• 생약학회지
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• 제39권3호
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• pp.199-202
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• 2008

A high performance liquid chromatographic (HPLC) method for the simultaneous determination of hesperidin and glycyrrhizin was established for the quality control of traditional herbal medicinal preparation, Pyungwi-san (PWS). Separation and quantification were successfully achieved with a Waters XTerra RP18 column ($5{\mu}m$, 4.6 mm I.D. ${\times}$ 150 mm) by gradient elution of a mixture of acetonitrile and water containing 0.03% phosphoric acid (pH 2.03) at a flow rate of 1.0 ml/min. The diode-array UV/vis detector (DAD) was used for the detection and the wavelength for quantification was set at 230 nm. The presence of hesperidin and glycyrrhizin in this extract was ascertained by retention time, spiking with each authentic standard and UV spectrum. All four compounds showed good linearity $(r^2>0.995)$ in a relatively wide concentration ranges. The R.S.D. for intra-day and inter-day precision was less than 7.0% and the limits of detection (LOD) were less than 60 ng. The mean recovery of each compound was 99.0-105.6% with R.S.D. values less than 4.0%. This method was successfully applied to the determination of contents of hesperidin and glycyrrhizin in three commercial products of PWS. These results suggest that the developed HPLC method is simple, effective and could be readily utilized as a quality control method for commercial PWS products.

• 한국환경보건학회지
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• 제42권1호
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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.

• 한국의학물리학회지:의학물리
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• 제29권3호
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• pp.92-100
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• 2018

The manufacturer of a linear accelerator (LINAC) has reported that the target melting phenomenon could be caused by a non-recommended output setting and the excessive use of monitor unit (MU) with intensity-modulated radiation therapy (IMRT). Due to these reasons, we observed an unexpected beam interruption during the treatment of a patient in our institution. The target status was inspected and a replacement of the target was determined. After the target replacement, the beam profile was adjusted to the machine commissioning beam data, and the absolute doses-to-water for 6 MV and 10 MV photon beams were calibrated according to American Association of Physicists in Medicine (AAPM) Task Group (TG)-51 protocol. To verify the beam data after target replacement, the beam flatness, symmetry, output factor, and percent depth dose (PDD) were measured and compared with the commissioning data. The difference between the referenced and measured data for flatness and symmetry exhibited a coincidence within 0.3% for both 6 MV and 10 MV, and the difference of the PDD at 10 cm depth ($PDD_{10}$) was also within 0.3% for both photon energies. Also, patient-specific quality assurances (QAs) were performed with gamma analysis using a 2-D diode and ion chamber array detector for eight patients. The average gamma passing rates for all patients for the relative dose distribution was $99.1%{\pm}1.0%$, and those for absolute dose distribution was $97.2%{\pm}2.7%$, which means the gamma analysis results were all clinically acceptable. In this study, we recommend that the beam characteristics, such as beam profile, depth dose, and output factors, should be examined. Further, patient-specific QAs should be performed to verify the changes in the overall beam delivery system when a target replacement is inevitable; although it is more important to check the beam output in a daily routine.

• Journal of Acupuncture Research
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• 제32권2호
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• pp.1-9
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• 2015

Objectives : The present study was an evaluation and standardization of herbal components in order to establish the efficacy and safety of Shinbaro pharmacopuncture. Methods : Among the raw materials of Shinbaro pharmacopuncture, the components Cibotii Rhizoma, Eucommiae Cortex, and Ledebouriellae Radix were assessed through ingredient verification experiments using thin-layer chromatography(TLC) and ultraviolet rays(UV) lamps. In addition, we standardized Acanthopanacis Cortex and Achyranthis Radix through validation using high performance liquid chromatograph-diode array detector(HPLC-DAD). Results : As result appeared a blue-white fluorescence under ultraviolet rays; changed to dark green after adding 1 % ferric chloride solution(due to Cibotii Rhizoma), and presented a yellow-green fluorescence when mixed with an ethyl ether under UV lamps by way of the ethyl ether layer, confirming Eucommiae Cortex. Ledebouriellae Radix was confirmed as dark brown spots at Rf values of 0.56 and 0.71 using TLC. Additionally, Acanthopanacis Cortex and Achyranthis Radix HPLC test results showed that linearity was $R^2{\geq}0.99$, and detection limit and quantitation limit were 0.23 to $1.29{\mu}g/mL$, and 0.71 to $3.90{\mu}g/mL$, respectively. Furthermore, precision and accuracy were confirmed to have relative standard deviation(RSD) values of 0.10 to 1.89 % and 96.19 to 103.72 %, respectively. Shinbaro pharmacopuncture did not have any overlapping or interference from other peaks in detection under the abovementioned analysis conditions. Conclusions : In conclusion, we confirmed that maintenance of Shinbaro pharmacopuncture validity was possible by means of quality control of Cibotii Rhizoma, Eucommiae Cortex, and Ledebouriellae Radix through ingredient identification and Acanthopanacis Cortex and Achyranthis Radix through high performance liquid chromatograph(HPLC) analysis. Further, we hope to contribute to the development strategy of herbal industry acupuncture.

• 한국식품저장유통학회지
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• 제23권7호
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• pp.1004-1011
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• 2016

본 연구에서는 국내산 대추나무의 잎과 열매의 flavonoid 배당체를 조사하기 위하여 선행 연구된 인용문헌을 바탕으로 대추나무, 묏대추나무, 야생대추나무 등 대추나무속(Zizyphus)에 따른 flavonoid의 화학적 정보 수집 및 정리하여 대추나무속의 flavonoid 라이브러리를 제작하였다. 각 flavonoid 개별성분은 UPLC-DAD-QTOF-ESI/MS를 사용하여 분석하였으며 제작된 라이브러리의 정보를 이용하여 국내산 대추나무로부터 총 6종의 flavonoid를 확인하였다. 이를 통하여 국내산 대추나무 잎의 주요 성분은 quercetin 배당체인 rutin임을 확인하였고, 특히 quercetin 3-O-robinobioside 및 isoquercitrin는 구축된 라이브러리를 바탕으로 대추나무 잎에서는 처음 확인된 것을 알 수 있었다. 본 연구와 같이 대추나무속 flavonoid의 화합물 정보를 포함하여 제작한 라이브러리는 선행된 연구와의 차이점 판단을 가능하게 할 것으로 사료된다.

• 분석과학
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• 제29권4호
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• pp.202-208
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• 2016

A novel and simple method for detecting seven organic acids (formic acid, malic acid, lactic acid, acetic acid, citric acid, fumaric acid and propionic acid) in animal feed using high performance liquid chromatography equipped with a photo-diode array detector (HPLC/PDA) was developed. The chromatographic peaks of the seven organic acids were successfully identified by comparing their retention times and UV spectra with reference standards. Method validation was performed in terms of linearity, sensitivity, selectivity, accuracy, and precision. The limits of detection (LODs) for the instrument employed in these experiments ranged from 12 to 8,026 μg/kg, and the limits of quantification (LOQs) ranged from 43 to 26,755 μg/kg. Average recoveries of the seven organic acids ranged from 79.3 to 95.2 %. Method replication resulted in intra- day and inter-day peak area variation of <3.2 %. The developed method was specific and reliable and is therefore suitable for the routine analysis of organic acids in animal feed.

• 한국식품위생안전성학회지
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• 제36권5호
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• pp.376-381
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• 2021

Red beet roots (Beta vulgaris L.)는 천연색소로 붉은 색계열의 betacyanins은 75-95%의 betanine와 이성질체인 isobetanine 15-45%으로 존재한다. 본 연구는 비트레드를 사용한 식품에 대해 HPLC-DAD를 이용하여 지표성분인 betanine 및 isobetanine에 대해 분석법을 확립하였으며, 유효성 검증을 위해 직선성, 검출한계, 정량한계, 정확성, 정밀성, 측정불확도를 측정하였다. 캔디류, 빙과류, 코코아 가공품의 matrix에 적용하여 matrix matched calibration법을 사용하였으며 R²이 0.9998 이상으로 높은 직선성을 보였다. 검출한계와 정량한계는 각각 0.16-0.32 mg/L, 0.48-0.97 mg/L으로 확인되었다. 분석법의 정확성 및 정밀성을 검증하기 위해 intra-day 및 inter-day 반복 실험 결과, 회수율은 96.0-103.1 %, 100.0-102.2 %이였으며, RSD는 0.5-3.3 %, 0.9-3.8 %로 산출되었다. 측정불확도는 매트릭스 및 측정 농도에 따라 1.71-12.43%로 평가되었다. 또한, 확립된 분석법의 적용성 검토를 위해서 비트레드 색소를 사용한 가공식품 26종을 분석한 결과, betanine과 isobetanine을 정량 할 수 있었다 (8.4-3,823.4 mg/kg).