• Journal of Korean Society of Environmental Engineers
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• v.28 no.2
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• pp.223-228
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• 2006

High-performance liquid chromatography(HPLC) and fluorescence derivatization were applied for a trace-level N-nitrosodimethylamine(NDMA) analysis of water samples. Fluorescence intensity was optimized with the excitation wavelength of 340 nm and the emission wavelength of 530 nm. pH adjustment after denitrosation was necessary to get a maximum intensity at pH between 9 and 12. Maximum intensity was found with a dansyl chloride concentration of 330 to 500 mg/L. Percentile error in the water sample analyses through solid phase extraction was 12-162% and 6-23% for the lower concentration level(10-200 ng/L NDMA) and the higher level(100-1000 ng/L NDMA), respectively, showing more discrepancy in lower level. However, the average ratios of estimated NDMA to the standard NDMA were close to 1 for both concentration ranges, presenting this HPLC method could detect from tens to hundreds nanograms NDMA per liter. Accurate determination of NDMA, which was injected to a wastewater effluent, revealed the selectivity of fluorescence derivatization for the target compound(NDMA) in the presence of complex interfering compounds. The HPLC with fluorescence derivatization may be applicable for determining NDMA of water and wastewater samples fur various research purposes.

• Journal of Environmental Health Sciences
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• v.22 no.1
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• pp.36-44
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• 1996

A comparison was made of two detection methods(UV absorbence detection and fluorescence detection with pre-column derivatization, with trifluoroacetic acid) coupled with HPLC for the simultaneous determination of aflatoxin $B_1, B_2, G_1$ and $G_2$. A good separation of the four aflatoxins was achieved on a reversed-phase $C_{18}$ column (30 cm x 3.9 mm) with methanol-acetonitrile-water(20+20+60) for absorbence detection or acetonitrile-water(25+75) for fluorescence detection at the flow rate of 1.0 ml/min. The calibration graphs were linear over the ranges 100 ppb-1 ppm for $B_1/G_1$ and 30~300 ppb for $B_2/G_1$ with absorbence detection, and 1~500 ppb for $B_1/G_1$ and 0.3~150 ppb for $B_2/G_2$ with fluorescence detection. The correlation coefficients were greater than 0.94 and 0.99 for absorbance detection and for fluorescence detection, respectively. The detection limit was 100 ng for $B_1/G_1$ and 30 ng for $B_2/G_2$ with absorbence detection, and 1 ng for $B_1/G_1$ and 0.3 ng for $B_2/G_2$ with fluorescence detection. Recovery rates of aflatoxin $B_1, B_2, G_1$ and $G_2$ added to yeast-extract sucrose broth medium were 66.6%, 59.4%, 67.5% and 59.2%, respectively, for absorbence detection and 82.9%, 71.5%, 80.0% and 69.3%, respectively, for fluorescence detection. The four aflatoxins in culture medium were quantitatively detected by the two methods. The aflatoxins in the rice sample were not detected the absorbence detection method, but were below 10 ppb using the fluorescence detection method. Analysis of aflatoxins by both the absorbence and fluorescence methods coupled with HPLC showed acceptable linearity and good recovery. The absorbence detection was less timeconsuming and safer for treatment. The fluorescence detection was more elective and sensitive though elevated $B_1$ and $G_1$ contents were determined from the TFA-induced conversion of $B_1$ to $B_{2a}$ and $G_1$ to $G_{2a}$.

• Journal of Life Science
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• v.23 no.2
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• pp.306-310
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• 2013

We compared the efficacy of the competitive ELISA method for measuring the level of urinary aflatoxin M1 (AFM1) with that of the HPLC-fluorescence detector (HPLC-FLD) method. The recovery rate of AFM1 with the ELISA method was 105% (73-124%), and the coefficient of variation of the analysis was 6.85%. The ELISA method showed a 0.20 pg/ml and 0.62 pg/ml limit of detection and limit of quantitation, respectively. In correlation analysis, the two methods showed a very strong and statistically significant correlation (R=0.96, p<0.01). However, in spite of the strong correlation, the ELISA method tended to overestimate the urinary AFM1 concentration compared to the HPLC-FLD method. These results suggest that the competitive ELISA method may be a useful technique for measuring the AFM1 level in high-throughput urine samples, but it needs to be corrected with a regression equation from regression analysis with the HPLC-FLD method.

• Journal of Soil and Groundwater Environment
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• v.14 no.6
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• pp.35-44
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• 2009

Naphthalene and TNT (2,4,6-trinitrotoluene) are defined by U.S. EPA as possible carcinogenic compounds known to have detrimental effects on the aquatic ecosystem and human body. There are, however, few researches on methods of analyzing micro-levels of naphthalene and TNT dissolved in groundwater. This study introduces and evaluates the newly developed analytical methods of measuring naphthalene and TNT in groundwater by using HPLC-FLD (Fluorescence detector) and MSD (Mass detector). The MDL, LOQ and salt effect of these methods, respectively, are compared with those of conventional methods which use HPLC-UV. For the analysis of naphthalene, HPLC-FLD was set in the maxima wavelength (Ex: 270 nM, Em: 330 nM) obtained from 3D-Fluorescence to be compared with HPLC-UV in 266 nM wavelength. The MDL ($0.3\;{\mu}g/L$) and LOQ ($2.0\;{\mu}g/L$) of naphthalene by using HPLC-FLD were approximately 80 times lower than those analyzed by HPLC-UV (MDL: $23.3\;{\mu}g/L$, LOQ: $163.1\;{\mu}g/L$). HPLC-MSD were used in comparison with HPLC-UV in 230 and 254 nM wavelength for the analysis of TNT. The MDL ($0.13\;{\mu}g/L$) and LOQ ($0.88\;{\mu}g/L$) of TNT analyzed by using HPLC-MSD were approximately 130 times lower than those obtained by using HPLC-UV in 230 nM (MDL: $16.8\;{\mu}g/L$, LOQ: $117.5\;{\mu}g/L$). The chromatogram of TNT analyzed by using HPLC-UV in 230 nM displayed elevated baseline as the concentration of ${NO_3}^-$ increases beyond 21 mg/L, while the analysis using HPLC-MSD did not demonstrate any change in baseline in presence of ${NO_3}^-$ of 63.7 mg/L which is 3.5 times higher than average concentration in groundwater. In conclusion, HPLC-FLD and HPLC-MSD may be used as suitable methods for the analysis of naphthalene and TNT in groundwater and drinking water. These methods can be applied to the monitoring of naphthalene and TNT concentration in groundwater or drinking water.

• YAKHAK HOEJI
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• v.45 no.4
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• pp.347-351
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• 2001

A rapid and sensitive method for the determination of glyphosate, a phosphated amino acid herbicide, in whole blood is presented. After removal of protein, the whale blood was purified by using the anion exchange resin (Dowex 1), and derivatized with 9-fluorenylmethyl chloroformate (FMCL). Derivatized glyphosate from blood sample was injected onto a Whatman partisil 10SAX column and separated with 0.1M phosphate buffer (pH 2.5) and acetonitrile (ratio=3:1). The high performance liquid chromatography-fluorescence detection gave the detection limit of 86pg and linearity of 0.9999 in the range of 0.25 $\mu$g/ml and 25 $\mu$g/ml. The recoveries of glyphosate added to the blood samples were ranged from 75.3% to 100.4% compared to the samples prepared in water. The derivatized glyphosate was stable at various acidity and temperature. This method has been successfully applied to the blood samples of lethal intoxication with the herbicide glyphosate.

• Archives of Pharmacal Research
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• v.19 no.6
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• pp.562-565
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• 1996

The photoreactivity of twelve anthraquinone derivatives was examined to evaluate its usefulness as a photo-reagent for the analysis of ginsenosides using photoreduction fluorescence (PRF) detection method. Among the tested compounds, 2-tert-butylandthraquinone (TBAQ), 2-chloroanthraquinone (CAQ) and anthraquinone (AQ) showed good characteristics as photoreagents. The detection limits of ginsenoside $Rg_{1}$PRF-HPLC method using TBAQ, CAQ or AQ as a photo-reagent were found to be ca. 35 ng, 50 ng and 50 ng, respectively.

• Analytical Science and Technology
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• v.16 no.6
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• pp.499-503
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• 2003

A high performance liquid chromatography gradient elution method with fluorescence detection for the determination of biotin in pure form and pharmaceutical preparations has been developed. BrMDMC gives intense fluorescence and the fluorescence was monitored with excitation at 360 nm and emission at 410 nm. The calibration curve for biotin shows good linearity over the range of 5 ~ 400 ng with correlation coefficient of 0.999. The detection limit of biotin was 2 ng and the result of recovery was 98.75% with relative standard deviation of 1.1%.

• YAKHAK HOEJI
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• v.40 no.1
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• pp.41-45
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• 1996

A high performance liquid chromatography using photoreduction fluorescence detection was described for the analysis of saikosaponins. Saikosaponins were separated on an $NH_2$ column using acetonitrile and aqueous 2-tert-butylanthraquinone(t-BAQ) as mobile phase. Column effluent was passed through a 40cm PTFE capillary tube coiled around a 10W UV lamp to reduce t-BAQ to a highly fluorescent dihydroxyanthracene derivative which was detected by a fluorescence detector. The optimal concentration of t-BAQ was found to be $6{\times}10^{-5}M$ and the optimal reaction time to be 2 seconds. The detection limit for saikosaponin a and d by this method was found to be about 280ng and 80ng. The dynamic linear range was over two orders and the correlation coefficient of the calibration curve of them was 0.998.

• Bulletin of the Korean Chemical Society
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• v.26 no.2
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• pp.268-272
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• 2005

Different detection characteristics of fluorescence immunochromatography method and high performance liquid chromatography (HPLC) method for the analysis of cyanobacterial toxins were studied. In particular, low and high limits of detection, detection time and reproducibility and detectable microcystin species were compared when fluorescence immunochromatography method and high performance liquid chromatography method were applied for the detection of microcystin (MC), a cyclic peptide toxin of the freshwater cyanobacterium Microcystis aeruginosa. A Fluorescence immunochromatography assay system has the unique advantages of short detection time and low detection limit, and high performance liquid chromatography detection method has the strong advantage of individual quantifications of several species of microcystins.

• YAKHAK HOEJI
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• v.37 no.1
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• pp.30-35
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• 1993

HPLC/fluorescence detection method for the analysis of pancuronium bromide in biological fluids was developed. The method depends on the formation of insoluble red complex between pancuronium bromide and rose bengal in aqueous layer. This complex is quantitatively extracted from aqueous layer into chloroform layer. The complex is stable for 1 day in chloroform layer at room temperature. It was possible to analyze pancuronium bromide in the range of 0.05~0.5 $\mu\textrm{g}$/ml without the effect of co-prescribed drugs.