• Fisheries and Aquatic Sciences
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• v.16 no.3
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• pp.159-164
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• 2013

The mouse bioassay and high performance liquid chromatography (HPLC) post-column oxidation method are different methods of quantifying paralytic shellfish poisoning toxins. In this study, we compared their ability to accurately quantify the toxicity levels in two types of field sample (oysters and mussels) with different toxin profiles for routine regulatory monitoring. A total of 72 samples were analyzed by both methods, 44 of which gave negative results, with readings under the limit of detection of the mouse bioassay ($40{\mu}g/100g$ saxitoxin [STX] eq). In 14 oysters, the major toxin components were gonyautoxin (GTX) 1, -2, -3, -4, -5, decarbamoylgonyautoxin-2 (dcGTX2), and decarbamoylsaxitoxin (dcSTX), while 14 mussels tested positive for dcSTX, GTX2, -3, -4, -5, dcGTX2, neosaxitoxin (NEO), STX, and dcSTX. When the results obtained by both methods were compared in two matrices, a better correlation ($r^2=0.9478$) was obtained for mussels than for oysters ($r^2=0.8244$). Additional studies are therefore needed in oysters to investigate the differences in the results obtained by both methods. Importantly, some samples with toxin levels around the legal limit gave inconsistent results using HPLC-based techniques, which could have a strong economic impact due to enforced harvest area closure. It should therefore be determined if all paralytic shellfish poisoning toxins can be quantified accurately by HPLC, and if the uncertainties of the method lead to doubts regarding regulatory limits.

• Journal of Korean Society of Environmental Engineers
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• v.37 no.5
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• pp.293-302
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• 2015

Halonitromethanes (HNMs) are one of the most toxic groups of disinfection by-products. Recently, various studies have been fulfilled. An automated headspace-solid phase microextraction (SPME) gas chromatography/electron capture detector (GC-ECD) technique was developed for routine analysis of 9 HNMs in water samples. The optimization of the method is discussed. The limits of detection (LOD) and limits of quantification (LOQ) range from 90 ng/L to 260 ng/L and from 270 ng/L to 840 ng/L for 9 HNMs, respectively. Matrix effects in tap water and sea water were investigated and it was shown that the method is suitable for the analysis of trace levels of HNMs, in a wide range of waters. The method developed in the present study has the advantage of being rapid, simple and sensitive.

• Natural Product Sciences
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• v.28 no.4
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• pp.187-193
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• 2022

Lysimachia christinae Hance was commonly used in Oriental medicine for treating the hepatitis virus, cholecystitis and cholagogic efficiency. According to the previous study, it possesses high antioxidant and anti-inflammatory activity. Simultaneous determination analytical method of isolated eight compounds, cynaroside (1), 2-(3,4-dimethoxyphenyl) ethyl O-α-L-arabinopyranosyl-(1→2)-O-[6-deoxy-α-L-mannopyranosyl-(1→3)] β-D-glucopyranoside (2), stearylester ricinoleic acid (3), (E)-4-(3,4-dimethoxyphenyl) but-3-en-1-yl palmitate (4), 2-hydroxy-24-methoxy-4-tetracosenoic acid (5), 2-hydroxy-24-propoxy-4-tetracosenoic acid (6), β-sitosterol (7), and androst-16-ene-3,6-diol (8) were established by using HPLC-DAD. This HPLC analysis was detected on a Dionex C18 column (5 ㎛, 120 Å, 4.6 mm × 150 mm) at 25℃. The mobile phase consisted of 0.1% trifluoroacetic acid and acetonitrile at a flow rate of 1 mL/min. Validation of the method was assessed by linearity, precision and accuracy test. Calibration curve was good at r² > 0.9998. Limits of detection (LOD) ranged from 0.19 to 8.18 g/ml and Limits of quantification (LOQ) ranged from 0.19 to 24.80 g/ml. The relative standard deviations (RSD) values of precision test, intra- and inter- day, were less than 0.99% and 1.0%. The accuracy test results ranged from 98.81% to 106.49% and RSD values were less than 0.95%. These results showed that the HPLC-DAD method was very reliable and accurate for the quantity analysis of eight compounds in L. christinae extract for quality control.

• Journal of Food Hygiene and Safety
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• v.34 no.3
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• pp.269-276
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• 2019

A colorimetric rapid detection method based on acetylcholinesterase (AChE) was developed for the analysis of organophosphorus (OP) and carbamate (CB) pesticides. The AChE catalyzes acetylthiocholine into thiocholine having (-) and (+) charges, and the (+) charge results in gold nanoparticle (GNP) aggregation. The in-activation of AChE by OP and CB has been well known. In order to optimize the colorimetric method, optimal dilution times of commercial serum containing AChE, diameter of GNP, and concentration of acetylthiocholine were tested as a key parameter. The colorimetric detection limits of the method were 7.5 ng/mL for both dimethyl amine and carbofuran pesticides in 60% ethanol. No cross-reaction to other chemicals, such as aflatoxin B1 and ochratoxin A, which can be contaminated with pesticides in agricultural products, was observed. Recoveries from lettuce, sesame leaf, and cabbage lettuce spiked with known concentrations of dimethyl amine and carbofuran were found to be ranged from 83.85 to 133.16%. These results indicated that the colorimetric rapid method based on AChE can be a useful tool for the sensitive, specific, rapid, and accurate detection of OP and CB pesticides in fresh vegetables.

• Journal of Korean Society for Atmospheric Environment
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• v.5 no.2
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• pp.21-29
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• 1989

The metals present in atmospheric particulate come from various sources; natural or anthropogenic. Among various metals Fe, Zn, Pb, Cu, and Mn are of particular concern in as much as they are not only present in large quantity, but toxic to human body. A simple, fast, and non-destructive analytical method for these metals in atmospheric particulate was developed and the analytical details were described herein. The method involves the measurements of X-ray fluorescence of sample contained in filters and comparing it with those for standards. The standard filters were prepared by applicating premeasured standard solution to the filters and then drying. The accuracy of the method was tested by analyzing standard reference materials and by independently analyzing samples using a different, previously accuracy-proven method, inductively coupled plasma atomic emission spectrometry, and comparing the results obtained. Analytical sensitivities and detection limits of the present method were 62.9, 178.2, 82.9, 146.1, 37.2, 120.3 cps/$\mug/cm^2$ and 39.0 35.6, 137.5, 125.9, 182.6, 72.8 $ng/cm^2$ for Fe, Zn, Pb, Cu, Mn, and Ni respectively. The method was applied to Seoul atmospheric particulate and some results were reported.

• Korean Journal of Food Science and Technology
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• v.32 no.3
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• pp.570-577
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• 2000

A method was presented for determination of bisphenol F(BPF), bisphenol A(BPA), bisphenol F diglycidyl ether(BFDGE) and bisphenol A diglycidyl ether(BADGE) in 3 aqueous-based food simulants (water, 4% acetic acid, 20% ethanol) by reverse-phase high performance liquid chromatography(RP-HPLC)with fluorescence detection and gas chromatography with mass selective detection(GC/MSD). All the calibration lines in the range of $5{\sim}800\;{\mu}g/L$ had correlation coefficients greater than 0.9998 and detection limits of less than $1.2\;{\mu}g$ bisphenols/L. Precision at $200\;{\mu}g/L$ was under 3.1%. Recoveries of bisphenols simultaneously spiked to aqueous food simulants exceeded 95% for BPF and BPA but about 80% for BFDGE and BADGE. However, recoveris of BFDGE and BPADGE respectively spiked increased upto 95%. Detection limits in recovery test were less than $0.40\;{\mu}g$ bisphenols/L. In migration test bisphenols were determined by RP-HPLC coupled with confirmation by GC/MSD. Can coatings of epoxy phenol, modified epoxy, epoxy ester phenol and thermoset vinyl were exposed to the 3 aqueous food simulants. BPF, BFDGE and BADGE were not detected in all the can coatings but BPA was detected in 4% acetic acid and 20% ethanol in all the can coatings except modified epoxy.

• Korean Journal of Food Science and Technology
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• v.43 no.1
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• pp.1-5
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• 2011

It is possible that veterinary medicines remain in livestock food products, according to the use of many and various veterinary medicines to protect against disease when livestock animals are breed in limited space. Concentrated and continuous monitoring of residues is needed due to increases in resistance to antibiotics and side effects by eating livestock food products. We developed an analysis method for detecting streptomycin, dihydrostreptomycin, neomycin, gentamicin and spectinomycin in meat using LC/MS/MS and measured sensitivity, precision, accuracy, linearity and recovery according to CODEX guidelines to acquire confidence in the analysis method. Based on the results, we acquired good sensitivity compared to the maximum residue limit (MRL) as limits of detection (LOD) were 0.002-0.016 mg/kg and limits of quantification (LOQ) were 0.006-0.050 mg/kg. The analysis method satisfied the CODEX guidelines. The linearity ($r^2$) values of aminoglycoside antibiotics were 0.9936-0.9980, recoveries were 60-110% and relative standard deviations (RSD) were within 15%. As a result of monitoring for residues in a total 250 samples of livestock foods such as pork, chicken, and beef by the confirmed method, dihydrostreptomycin and gentamicin were detected in 5 pork samples. The residues of these antibiotics were within the MRLs. Thus, the detection ratio was 2% as 5 samples were identified from 250 samples.

• Journal of Korean Society of Environmental Engineers
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• v.36 no.11
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• pp.764-770
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• 2014

This study assessed analysis of N-nitrosamines by separation, identification, and quantification using a gas chromatography (GC) mass spectrometer (MS) with electron impact (EI) mode. Samples were pretreated by a automated solid phase extraction (SPE) and a nitrogen concentration technique to detect low concentration ranges. The analysis results by EI-GC/MS (SIM) and EI-GC/MS/MS (MRM) on standard samples with no pretreatment exhibited similar results. On the other hand, the analysis of pretreated samples at low concentrations (i.e. ng/L levels) were not reliable with a EI-GC/MS due to the interferences from impurity peaks. The method detection limits of eight (8) N-nitrosamines by EI-GC/MS/MS analysis ranged from 0.76 to 2.09 ng/L, and the limits of quantification ranged from 2.41 to 6.65 ng/L. The precision and accuracy of the method were evaluated using spiked samples at concentrations of 10, 20 and 100 ng/L. The precision were 1.2~13.6%, and the accuracy were 80.4~121.8%. The $R^2$ of the calibration curves were greater than 0.999. The recovery rates for various environmental samples were evaluated with a surrogate material (NDPA-$d_{14}$) and ranged 86.2~122.3%. Thus, this method can be used to determine low (ng/L) levels of N-nitrosamines in water samples.

• Food Science of Animal Resources
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• v.32 no.5
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• pp.571-577
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• 2012

This study was carried out to develop an analytical method for the determination of vitamin D in infant formula. Vitamin D was determined by column-switching high-performance liquid chromatography (HPLC) equipped with a reversed phase column and UV detector after saponification and extraction of the formula with an organic solvent. A preseparation column ($C_8$), focusing column ($C_{18}$), analytical column ($C_{18}$) and UV-Vis detector (254 nm) were used. The limits of detection (LOD) and the limits of quantification (LOQ) for vitamin D were estimated to be $1.51{\mu}g/kg$ and $4.95{\mu}g/kg$, respectively. The linearity, recovery, precision and accuracy of the analytical method for vitamin D were evaluated through the application of a SRM (Standard Reference Material) 1846 (National Institute of Standard & Technology, USA). The linearity of this method was calculated with a value of the coefficient of determination ($r^2$) ${\geq}0.9999$. The recovery of vitamin D was $85.20{\pm}3.00%$. The intra-assay precision for vitamin D was between $1.68{\pm}0.03%$ and $5.75{\pm}0.33%$, and the inter-assay precision for vitamin D ranged from $1.73{\pm}0.03%$ to $2.96{\pm}0.09%$. The intra-assay accuracy for vitamin D was between $100.03{\pm}2.77%$ and $102.01{\pm}0.59%$, and the inter-assay accuracy for vitamin D ranged from $99.00{\pm}1.53%$ to $102.01{\pm}3.04%$. The proposed method is optimal for the separation and quantification of vitamin D from infant formula.

• Journal of Soil and Groundwater Environment
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• v.14 no.2
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• pp.45-53
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• 2009

A quick and simple detection method of explosive compounds in environmental matrix (soil and water) can provide a screening step which reduces the number of unnecessary samples and the cost of expensive laboratory analysis at a site investigation. A commercially available EXPRAY$^{(R)}$Explosives Field Detection Kit (EXPRAY) was used to determine the minimum detection concentration and to test the possibility of semi-quantitative analysis of 14 explosive compounds using standard solutions. The results showed that EXPRAY could detect 5 explosive compounds, TNT, RDX, HMX, Tetryl, and TNB, out of 14 US EPA designated explosives. The minimum detection limit of the nitramine explosives was 14 ng/$^2$ for HMX and RDX. EXPRAY was more sensitive to nitroaromatics than the nitramines and the minimum detection limits per unit area (mm$^2$) for Tetryl, TNB, and TNT, were 3 ng, 3 ng, and 0.3 ng, respectively. The semi-quantification of 5 explosive compounds in an order ofmagnitude could be achieved by the intensity of developed color only when EXPRAY was applied on the standard solutions under controlled laboratory conditions. With contaminated soil samples, however, only the presence and type of explosive compounds was identified. Therefore, EXPRAY is an economic and sensitive method that can be used in a screening step for the identification of explosives in the field samples.