• Korean Journal of Food Science and Technology
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• v.42 no.4
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• pp.383-389
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• 2010

The aim of this study was to determine the methylmercury (MeHg) levels in abyssal fish species. The MeHg in the fishes was extracted with hydrochloric acid and toluene and then purified using an L-cysteine solution. The extract was analyzed with a gas chromatography-electron capture detector (GC-${\mu}ECD$) with a thermon Hg-capillary column. The detection limit and the recovery of the method were 0.002 and 84.2-98.5% (mean, 93.4%), respectively. The MeHg content in 492 abyssal fishes ranged from 0.037 to 2.009 mg/kg. The levels of MeHg [range, mg/kg (mean)] were significantly dependent on fish species and presented as the following; 0.157-2.009 (0.546) in Scalloped hammerhead shark, 0.211-0.878 (0.501) in Blue shark, 0.121-0.993 (0.482) in Spiny dogfish, 0.243-0.658 (0.397) in Salmon shark, 0.074-1.958 (0.353) in Blacktip shark, 0.038-0.807 (0.302) in Southern hake, 0.099-0.511 (0.300) in Scorpion fish, and 0.037-0.133 (0.067) in Ling. The monitoring results showed that the estimated weekly intake of MeHg from sharks, Southern hake, and Ling were lower than the provisional tolerable weekly intake recommended by the Joint FAO/WHO expert committee on food additives.

• Korean Journal of Food Science and Technology
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• v.37 no.6
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• pp.882-888
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• 2005

Procedure for analysis of methylmercury in fish was developed, involving addition of HCl, extraction with toluene, and clean-up using L-cystein solution. Obtained extract is analyzed by gas chromatography with electron capture detector using Ulbon HR-Thermon-Hg column. Detection limit and recovery of the method were 0.005mg/kg (expressed as Hg), 98-107 (103%), respectively. Total mercury and methylmercury concentrations in 175 commercial fish samples ranged from [mean-max (mean), unit: mg/kg]: 0.014-1.200 (0.270) and 0.006-0.901 (0.168) in tuna-fish, 0.020-0.934 (0.323) and 0.012-0.553 (0.149) in martin-fish, 0.082-0.782 (0.391) and 0.040-0.436(0.201) in shark, 0,023-0.031 (0.026) and 0,013-0.018 (0.015) in salmon, 0.098-0.193 (0.133) and 0.031-0.015(0.090) in tilefish, and 0,031-0.214 (0.089) and 0.016-0.093 (0.042) in canned tuna respectively. No sample of analyzed fish exceeded 1.0mg/kg wet wt., limit for methylmercury established by Codex. In all species examined, estimated weekly intake was lower than Provisional Tolerable Weekly Intake recommended by the JECFA (the Joint FAO/WHO Expert Committee on Food Additives).

• Korean Journal of Food Science and Technology
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• v.40 no.2
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• pp.123-128
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• 2008

The MRLs (maximum residue limits) of DDT (DDD and DDE) in fresh ginseng, dried ginseng, and steamed red ginseng are set as low as 0.01 mg/kg, 0.05 mg/kg, and 0.05 mg/kg, respectively. Therefore, this study was undertaken to develop a simple and highly sensitive analysis method, as well as to reduce interfering ginseng matrix peaks, for the determination of DDT isomers (o,p'-DDE, p,p'-DDE, o,p'-DDD, p,p'-DDD, o,p'-DDT, and p,p'-DDT) in fresh ginseng, dried ginseng, and steamed red ginseng at the 0.01 mg/kg level. The method used acetonitrile extraction according to simultaneous analysis, followed by normal-phase Florisil solid-phase extraction column clean-up. The purification method entailed the following steps: (1) dissolve the concentrated sample extract in 7 mL hexane; (2) add 3 mL of $H_2SO_4$; (3) vigorously shake on avortex mixer; (4) cetrifuge at 2000 rpm for 5 min; (5) transfer 3.5 mL of the supernatant to the Florisil-SPE (500 mg/6 mL);and (6) elute the SPE column with 1.5 mL of hexane and 10 mL of ether/hexane (6:94). The determination of DDT isomers was carried out by a gas chromatography-electron capture detector (GC-${\mu}$ECD). The hexane and ether/hexane (6:94) eluate significantly removed chromatographic interferences, and the addition of 30% $H_2SO_4$ to the acetonitrile extract effectively reduced many interfering ginseng matrix peaks, to allow for the determination of the DDT isomers at the 0.01 mg/kg level. The recoveries of the 6 fortified (most at 0.01 mg/kg) DDT isomers from fresh ginseng, dried ginseng, and steamed red ginseng ranged from 87.9 to 99.6%. The MDLs (method detection limits) ranged from 0.003 to 0.009 mg/kg. Finally, the application of this method for the determination of DDT isomers is sensitive, rapid, simple, and inexpensive.

• Korean Journal of Environmental Agriculture
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• v.32 no.3
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• pp.214-223
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• 2013

BACKGROUND: This study focused on the development of an analytical method about dichlorprop (DCPP; 2-(2,4-dichlorophenoxy)propionic acid) which is a plant growth regulator, a synthetic auxin for agricultural commodities. DCPP prevents falling of fruits during their growth periods. However, the overdose of DCPP caused the unwanted maturing time and reduce the safe storage period. If we take fruits with exceeding maximum residue limits, it could be harmful. Therefore, this study presented the analytical method of DCPP in agricultural commodities for the nation-wide pesticide residues monitoring program of the Ministry of Food and Drug Safety. METHODS AND RESULTS: We adopted the analytical method for DCPP in agricultural commodities by gas chromatograph in cooperated with Electron Capture Detector(ECD). Sample extraction and purification by ion-associated partition method were applied, then quantitation was done by GC/ECD with DB-17, a moderate polarity column under the temperature-rising condition with nitrogen as a carrier gas and split-less mode. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.9998, analysed from 0.1 to 2.0 mg/L concentration. Limit of quantitation in agricultural commodities represents 0.05 mg/kg, and average recoveries ranged from 78.8 to 102.2%. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 9.5% in 0.05, 0.10, and 0.50 mg/kg. CONCLUSION(S): Our newly improved analytical method for DCPP residues in agricultural commodities was applicable to the nation-wide pesticide residues monitoring program with the acceptable level of sensitivity, repeatability and reproducibility.