• 청정기술
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• 제15권2호
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• pp.81-90
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• 2009

본 연구에서는 산업체에서 대체 세정제를 객관적이고 체계적으로 선정하는데 도움을 주고자 여러 가지 세정성 평가방법을 실험을 통하여 비교 평가하였다. 세정성 평가방법으로는 중량법, OSEE (optically simulated electron emission)법, 접촉각법과 FTIR, UV-VIS, HPLC와 같은 정밀분석기기를 이용한 분석법을 사용하여 flux, solder, grease 등의 오염물질에 대한 세정성 평가를 수행하였다. 그 결과 중량법은 쉽고 간단하게 세정제의 세정효율을 측정할 수 있었지만 중량측정의 한계로 정밀측정이 어려웠다. 반면에 OSEE법은 세정제의 세정성 평가를 빠르고 정밀하게 수행할 수 있었다. 접촉각 측정법은 피세정물 표면에 오염물질과 세정제에 의한 얇은 친유성 막의 형성으로 인하여 접촉각 변화에 영향을 주기 때문에 세정성 평가에 특별한 주의가 요구되었다. 중량법으로 수행하기 어려운 정밀세정성 평가의 경우 UV-VIS, FTIR, HPLC와 같은 정밀분석기기를 이용하여 피세정물에 잔류한 flux, solder, grease 등의 극미량의 오염물을 특수 용제로 추출하여 아주 작은 농도의 오염물을 정량분석할 수 있었다.

• 대한약침학회지
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• 제11권2호
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• pp.87-95
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• 2008

Objectives The aim of this experiment is to provide an differentiation of ginseng, red ginseng, cultivated wild ginseng(CWG), and red wild ginseng(RWG) through component analysis using HPLC(High Performance Liquid Chromatography, hereafter HPLC). Methods Comparative analyses of ginsenoside $Rg_3$, ginsenoside $Rh_2$, and ginsenosides $Rb_1$ and $Rg_1$ of various ginsengs were conducted using HPLC. Results 1. CWG was relatively heat-resistant and showed slow change in color during the process of steaming and drying, compared to cultivated ginseng. 2. Ginsenoside $Rg_3$ was not detected in cultivated ginseng and CWG, whereas it was high in red ginseng and RWG. Ginsenoside $Rg_3$ was more generated in red ginseng than in RWG. 3. Ginsenoside $Rh_2$ appreared during steaming and drying of cultivated ginseng, whereas it was more increased during steaming and drying of CWG. 4. Ginsenoside $Rg_1$ content was more increased during steaming and drying of cultivated ginseng, whereas it was more decreased during steaming and drying of CWG. 5. Ginsenoside $Rb_1$ content was increased about 500% during steaming and drying of cultivated ginseng, whereas it was increased about 30% during steaming and drying of CWG, indicating that ginsenoside $Rb_1$ was more generated in red ginseng than in RWG. 6. Ginsenoside $Rg_3$ content was higher, whereas ginsenoside $Rg_1$ content was lower in 11th RWG than in 9th RWG, indicating that ginsenoside $Rg_3$ content was increased and $Rg_1$ content was decreased as steaming and drying continued to proceed. Ginsenoside $Rh_2$ and $Rb_1$ contents began to be increased, followed by decreased after 9th steaming and drying process. Conclusions Above experiment data can be an important indicator for the dentification of ginseng, red ginseng, CWG, and RWG. And the following studies will be need for making good product using CWG.

• 한국작물학회지
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• 제50권spc1호
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• pp.1-3
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• 2005

흑자색미의 C3C함량을 신속하게 분석하는데, FT-NIR을 이용한 C3G 함량 분석의 예측값과 HPLC 측정값의 정확도를 비교하였다. 1. FT-NIR을 이용한 C3G 함량 분석에서 사용된 시료는 별도의 전처리 과정없이 현미 상태 측정하여 HPLC 분석방법에 비하여 많은 시간과 비용을 아낄 수 있다. 2. 흑진주벼와 수원425호를 교배한 $F_{10}$ 385 계통을 사용하여 얻은 FT-NIR 검량식은 매우 높은 정상관을 보였다($R^2=0.943$, SEE=0.116). 이 검량식을 검증한 결과도 매우 높은 정상관을 보이고 실험오차도 매우 적어($R^2=0.928$, SEP=0.122) 측정정확도가 높게 평가되었다. 3. 본 연구의 결과, FT-NIR을 이용하여 비파괴적으로 신속하게 흑자색미의 C3G함량을 측정할 수 있게 되었다. 그리고 본 연구의 결과를 C3G함량이 높은 벼를 개발하는데 많은 양의 시료를 빠르게 분석할 수 있는 방법으로 이용할 수 있을 것이다.

• 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.

• 대한약침학회지
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• 제12권4호
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• pp.33-50
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• 2009

Objectives : This study was conducted to confirm validation and stability of concentration analysis method of pure melittin (Sweet Bee Venom-Sweet BV) extracted from the bee venom by utilizing protein isolation method of gel filtration. Methods : All experiments were conducted at Biotoxtech, a non-clinical studies authorized institution, under the regulations of Good Laboratory Practice (GLP). Standard solutions of melittin (SIGMA, USA) and test substances were dispensed and were analyzed with HPLC for Sweet BV to secure the validation of analysis. Results : 1. Measurement of system suitability of Sweet BV satisfied criterion of below 3%. 2. Confirming Linearity of Sweet BV in 10-200${\mu}g/m\ell$ solution yielded correlation coefficient (r) of 0.995 and accuracy of 85-115% which satisfy criterion. 3. Measurement of Specificity of Sweet BV didn't yield any substance affecting the peak of test substances, but detected at 21.22min verified as the test substance. 4. Confirming Intra-day of Sweet BV, accuracy and precision of 0.1, 100${\mu}g/m\ell$ were 105.70, 95.81 and 0.66, 0.73, respectively, satisfying both criteria of accuracy (85-115%) and precision (within 10%). 5. To measure Stability in autosampler, all samples used in Intra-day reproducibility sat in the autosampler for five hours and were re-analyzed. Both variability and precision satisfied the criteria. 6. Homogeneity of Sweet BV (0.1, 100${\mu}g/m\ell$) at upper, middle, and lower layers all satisfied the accuracy and precision criteria. 7. Stability of Sweet BV (0.1, 100${\mu}g/m\ell$) at room temperature for four hours and refrigerated for 7 days all satisfied the criterion. 8. For the measurement of Quality control, QC samples measured on the first and eighth day all satisfied accuracy and precision criteria. Conclusion : Above experiment data satisfies validation and stability of concentration analysis method of Sweet BV.

• 분석과학
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• 제7권3호
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• pp.395-402
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• 1994

본 연구에서는 두 종류의 기존 HPLC 베노밀 분석법 및 한 종류의 새로이 설정한 GC PFB 유도체화 베노밀 분석법을 도입하여 시중에 유통되는 국산 및 수입작물을 수거한 후 그 잔류도를 검색함과 동시에 각 분석법의 정확성, 정밀도, 회수율, 그리고 감도 등을 비교 평가하였다. 그 결과 GC PFB 유도체화분석법의 경우 회수율 및 검출 한계가 각각 95% 이상, $0.001{\mu}g/g$이었다. 그리고 각종 작물의 분석시 기존의 HPLC법의 경우 베노밀의 peak가 나타나는 retention time 시간대에 시료의 성분에 의한 peak도 동시에 나타날 수 있는 확률이 높아 오검출되는 사례가 많았으나 GC PFB 유도체화분석법은 베노밀을 유도체화한 후 GC에서 분석함으로써 오검출 판정결과를 보이는 시료는 없었다.

• Asian Pacific Journal of Cancer Prevention
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• 제16권13호
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• pp.5211-5217
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• 2015

Background: We earlier used PCR-dHPLC for mutation analysis of BRCA1 and BRCA2. In this article we report application of targeted resequencing of 30 genes involved in hereditary cancers. Materials and Methods: A total of 91 patient samples were analysed using a panel of 30 genes in the Illumina HiScan SQ system. CLCBio was used for mapping reads to the reference sequences as well as for quality-based variant detection. All the deleterious mutations were then reconfirmed using Sanger sequencing. Kaplan Meier analysis was conducted to assess the effect of deleterious mutations on disease free and overall survival. Results: Seventy four of the 91 samples had been run earlier using the PCR-dHPLC and no deleterious mutations had been detected while 17 samples were tested for the first time. A total of 24 deleterious mutations were detected, 11 in BRCA1, 4 in BRCA2, 5 in p53, one each in RAD50, RAD52, ATM and TP53BP1. Some 19 deleterious mutations were seen in patients who had been tested earlier with PCR-dHPLC [19/74] and 5/17 in the samples tested for the first time, Together with our earlier detected 21 deleterious mutations in BRCA1 and BRCA2, we now had 45 mutations in 44 patients. BRCA1c.68_69delAG;p.Glu23ValfsX16 mutation was the most common, seen in 10/44 patients. Kaplan Meier survival analysis did not show any difference in disease free and overall survival in the patients with and without deleterious mutations. Conclusions: The NGS platform is more sensitive and cost effective in detecting mutations in genes involved in hereditary breast and/or ovarian cancers.

• 한국산업보건학회지
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• 제9권2호
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• pp.167-176
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• 1999

A new analytical procedure for the measurement of monomeric isocyanates and total isocyanate group in workplaces has been investigated. The method described herd involves derivatization of the isocyanate sample upon collection with the reagent 9-anthracenylmethyl 1-piperazinecarboxylate (PAC). Laboratory investigations have demonstrated that excess PAC reagent can be satisfactorily removed from PAC-derivatized monomeric isocyanates-a requirement for the success f the analytical procedure. After removal of excess PAC reagent, the PAC derivatives of butyl isocyanate, phenyl isocyanate, HDI, MDI, and TDI were reacted with sodium thiomethoxide to convert them all to 9-anthracenylmethyl methyl sulfide (AMMS). Total isocyanate group was determined by HPLC analysis and quantification of the single AMMS peak. This circumvents many of the disadvantages associated with current HPLC methods. There were no longer problems associated with quantifying late-eluting peaks and analysis times were very short. A single detector was used for quantification because a standard of the analyte existed and the retention time could be determined. Because all species were converted to a single analyte, the problem of variability of response factors among different species was averted. Finally, there were no complex chromatograms to interpret. Monomers of other individual species were measured by analysis of the sample before the individual species were converted to AMMS. The favorable performance of PAC warrants its further study as a reagent for the determination of total isocyanate group in air.

• 대한본초학회지
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• 제23권3호
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• pp.67-72
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• 2008

Objectives : This study presents a high performance liquid chromatography methods for the quantitative and qualitative analysis of rosmarinic acid (RA) and caffeic acid (CA) in Perilla frutescens var. japonica and var. acuta. Methods : Chromatographic separation was performed using a mixture of methanol, water and formic acid (35 : 64.2 : 0.8) with a reversed-phase column (Gemini C18, 4.6 ${\times}$ 150 mm, 3 ${\mu}m$). The analyses were detected at UV (280 nm). Results : The samples were extracted with 50% EtOH under reflux for 1 h, and simultaneous determination for RA and CA in hyang-so-san and haeng-so-san was possible without interference peaks Conclusions : According the results, we developed a determination method for RA and CA in Perillae Folium. Owing to Perilla frutescens var. japonica and var. acuta did not show significant difference in contents of RA and CA, both Perilla frutescens could be available as herbal medicine.

• 한국환경농학회지
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• 제30권3호
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• pp.288-294
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• 2011

최근에는 전처리가 단순하며 정량 시 방해물질의 영향을 최소화하기 위해 액체크로마토그래피를 이용하여 메틸수은을 분리한 후 유도결합플라즈마/질량분석기로 part per billion 수준까지 정량하는 방법들의 연구가 활발하다. 하지만 대부분의 액체크로마토그래피-유도결합플라즈마/질량분석기는 메틸수은 분리 시 전처리 용액의 pH를 조절하지 않으면 피크깨짐 등의 문제가 발생하여 pH를 조절하고 있다. 본 연구에서는 어류에 잔류하는 메틸수은을 신속하고 정확하게 분석하기 위하여 마이크로웨이브를 이용한 전처리 방법, HPLCICP/MS 조건, 시험법 검증의 실험을 통하여 효율적인 분석법을 확립하였다. 전처리 방법은 추출용매 1% L-cysteine HCl로 추출온도 $60^{\circ}C$에서 추출시간 120분 동안 추출하는 최적 조건을 확립하였다. 기기조건 중 HPLC에서는 시료주 입량 $50{\mu}L$, 컬럼온도는 $25^{\circ}C$에서 0.1% L-cysteine HCl + 0.1% L-cysteine 이동상으로 메틸수은을 분리 한 후, ICP-MS에서 분자량 202의 분석물질을 정량하는 조건을 확립하였다. 직선성에 대한 상관계수 값은 0.9998 이였으며, 검출한계 및 정량한계는 각각 0.15, $0.45{\mu}g/kg$ 이었다. 확립된 전처리 및 기기조건을 통하여 시료별 회수율을 구한 결과 95~99%였다. 전처리 용매와 이동상에 L-cysteine이 존재함으로써 수은에 대한 안정성, Memory effect 및 피크 끌림 등의 문제를 해결할 수 있었다. 확립된 HPLC-ICP/MS 방법에 대해 표준인증물질을 이용하여 검증한 결과, 회수율 및 상대표준편차가 각각 93~96%, 1~3%였다. 확립된 방법은 추출과정 후 별도의 전처리 과정 없이 바로 HPLC-ICP/MS를 이용하여 검출할 수 있어 메틸수은을 분석하기에 매우 적합한 것으로 판단된다.