• Korean Journal of Environmental Agriculture
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• v.31 no.3
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• pp.277-285
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• 2012

BACKGROUND: For safety evaluation of imported agri-food in Korea, the multiresidue analysis method was establised for unregistered organophosphorus pesticides, aspon, chlorthion, chlorthiophos, crotoxyphos, demeton-O, demeton-S, demeton-S-methyl, dioxathion, heptenophos, iodofenphos, leptophos, methyl-trithion, propetamphos and sulfotep. METHODS AND RESULTS: The used method for multiresidue analysis in brown rice and orange used as representative samples of imported agri-food was the official method of Korean Food and Drug Administration. The results of validation test of 13 organophosphorus pesticides except crotoxyphos for multiresidue analysis method are compared to the criteria such as specificity, linearity, accuracy, precision and limit of quantification. CONCLUSION: The used method for multiresidue analysis of unregistered 13 organophosphorus pesticides except crotoxyphos in Korea can surely be used as an official method for routine analysis of imported agri-food.

• Journal of Applied Biological Chemistry
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• v.42 no.4
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• pp.191-196
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• 1999

A multiresidue analytical method was developed for eight acaricides including benzoximate, clofentezine, fenazaquin, fenothiocarb, fenpyroximate, hexythiazox, pyridaben, and tebufenpyrad in four major fruits using high-performance liquid chromatography (HPLC). All the confounds were extracted with acetone from apple, pear, grape, and citrus samples. The extract was diluted with saline water, and n-heaxane partition was followed to recover the acaricides. Florisil column chromatography was employed to further purify the sample extract. HPLC with ultraviolet absorption detection, using an octadecylsilyl column under the isocratic mobile phase of acetonitrile/water mixture, was successfully applied to separate and quantitate all the compounds in the purified extract. Recoveries of the eight acaricides from for fortified samples ranged 86.4~97.0%. Relative standard deviations of the analytical method were all less than 10%. Detection limits of the method were in the range of 0.02~0.05 mg/kg. The proposed method was reproducible and sensitive enough to evaluate the terminal residue of the eight acaricides in the fruit harvest.

• Korean Journal of Environmental Agriculture
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• v.18 no.2
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• pp.154-163
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• 1999

A multiresidue method(MRM) for pesticides must be rapid and must test a wide variety of pesticides at relevant toxicological concentrations. In this study, three kinds of major analytical methods such as Korean Food Code Method, CDFA MRM, and Holstege's method are tested to compare the average recoveries, solvent consumption, and required time for the analysis of 18 organochlorines, 18 organophosphates, and 6 carbamates in spinach samples. Samples for pesticides analysis were extracted and cleaned up according to the respective methods and detected by gas chromatography with selective detectors, ECD and NPD, HPLC with postcolumn reaction system(PCRS). Average recovery of 42 pesticides by Korean Food Code method, CDFA method, and Holstege's method were 91.3%, 88.1%, 89.0%, respectively. Amount of solvent consumption and required time for the analysis of Korean Food Code method were from two and a half times to three times as much as those of another two methods. For the development and legal application of more rapid and effective MRMs, prolonged study is necessary.

• Korean Journal of Environmental Agriculture
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• v.23 no.3
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• pp.158-169
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• 2004

For the improvement of gas chromatographic analysis of multiple pesticide residues in green pepper, lettuce and Chinese cabbage, multiresidue test mixtures (MRTMs) of 10 groups (ECD 5 groups and NPD 5 groups) and a recovery test mixture (RTM) of 18 compounds (11 compounds for ECD and 7 compounds for NPD) were established based on retention time and response to relevant detectors. A new extraction solvent (acetone: acetonitrile=1 : 9) and a clean up eluent (hexane: dichloromethane : acetonitile = 50 : 48.5 : 1.5) for solid-phase extraction (SPE) cartridge were selected to test two types of multiresidue methods (MRM I and MRM II). MRM II provided high recovery better than MRM I when RTM was tested Recovery experiment with MRTMs which was conducted using MRM II resulted in that more than seventy percents of compounds were recovered in the range of $50{\sim}140%$, while 9% of compounds were over 140% of recovery and only $7{\sim}8$ compounds failed to detect. MRM II, an improved method, could be employed for screening residues of 190 pesticides in those vegetables.

• Environmental Analysis Health and Toxicology
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• v.17 no.3
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• pp.265-272
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• 2002

This study was carried out with the detection for multiresidue of the organophosphorus pesticides such as malathion, parathion. diazinon, and carbamate pesticide such as carbaryl, by enzyme-inhibition method. The acetylcholinesterase (AChE) and cholinesterase (ChE) activities in chicken brain determined by the Ellman's method were 166.6 and 5.8 $\mu$mol/min/g protein, and in chicken plasma were 23.1 and 8.3 $\mu$mol/min/g protein, respectively. The optimum pH of AChE and ChE was 8.2 and 7.8, respectively. The Km of AChE and ChE was 0.034 and 0.045 mM, respectively. I$\_$50/ for AChE and ChE by some organophosphorus was 55.82 and 99.42 mg/L of malathion, 31.16 and 29.13 mg/L of parathion, and 17.89 and 19.62 mg/L of diazinon, respectively. I$\_$50/ for AChE and ChE by carbaryl of carbamate was 0.10 and 0.05 mg/L, respectively. The 0.07 mg/L of drinking water advisory level for carbaryl could be detected with I$\_$50/ of AChE and ChE. Enzyme-Inhibition (EI) method with AChE and ChE was used the multiresidue method to detect the 1 mg/L of the carbamate pesticides.

• Journal of Soil and Groundwater Environment
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• v.11 no.4
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• pp.18-24
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• 2006

The possibility of multiresidue analysis of 24 pesticides out of 30 residual pesticides which are subjected to test in the golf courses was examined. The utility of multiresidue method for pesticide residue test was evaluated by recovery test through a standard addition method of pesticides in water, soil, and lawn grass. The experimental results of the recovery test for individual pesticides are as follows : The number of pesticide of which average recovery rate was over 70% regardless of media was 16 pesticides. These pesticides were composed of 8 organophosphorus pesticides (chlorpyrifos, chlorpyrifosmethyl, diazinon, EPN, fenitrothion, phenthoate, phosalone, and toclofos-methyl). 4-organochlorinated pesticides (daconil, captan, endosulfan, and tetradifon), 2-pyrethroid pesticides(fenpropathrin, lambda-cyhalothrin) and 2 other pesticides (bromopropylate, pendimethalin). On the other hand, in case of dicofol, average recovery rate was over 70% for water and lawn grass but only 53.3% for soil. Therefore, the multiresidue method applied in this experiment is not appropriate for analysis of dicofol in soil. Furthermore, among 7 pesticides, 2 pesticides(amitraz and pyraclofos) showed that theirs average recovery rate deviated from criteria($70{\sim}130%$) in almost ail media, while 5 pesticides(bensulide, deltamethrin, iprodione, phosphamidon and tralomethlin) were not detected from all media by GC/NPD or GC/ECD.

• Journal of Food Hygiene and Safety
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• v.30 no.4
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• pp.366-371
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• 2015

This work was conducted to apply the multi class pesticide multiresidue method for determining the use of hexaconazole in the agricultural products using GC-NPD. The multi class pesticide multiresidue method results were validated for the assay of hexaconazole by using linearity, accuracy, precision, limit of detection and quantitation. The linearity in the concentration ranged from 0.025 to 5.0 mg/L ($R^2$ > 0.999). Lettuce recoveries ranged from 89.42% to 94.15% with relative standard deviations below 7.78%, for spiking levels from 0.04 to 4.0 mg/kg. The limit of detection was 0.04 mg/kg, and the limit of quantitation was 0.11 mg/kg. The intra- and inter-day precisions were 2.42~3.49% and 4.90~7.78%, respectively. We suggested that the multi class pesticide multiresidue method for determining hexaconazole was highly accurate and reproducible, and it will be used as a routine analysis in agricultural products.

• Korean Journal of Environmental Agriculture
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• v.21 no.2
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• pp.90-95
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• 2002

A study was carried out to optimize the cleanup step using a solid-phase extraction (SPE) cartridge, $SupelClean^{TM}$ Florisil, for multiresidue analysis of 16 pesticides in cucumber matrix. Eluting efficiencies of two solvent systems including acetone/n-hexane and ethyl acetate/n-hexane mixtures were critically evaluated by recoveries of target anaytes from the SPE Florisil column. Based on the recovery as a measure of eluting efficiency, an acetone/n-hexane (20/80,v/v) mixture provided more than 80% recovery for 15 pesticides except bifenthrin. In case of ethyl acetate/n-hexane, 14 pesticides showed recoveries higher than 75% while those far alachlor and bifenthrin were less than 30%.

• Korean Journal of Food Science and Technology
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• v.37 no.2
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• pp.304-307
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• 2005

Multiresidue method was set up for the simultaneous determination of various residual pesticides in potatoes and carrots, which was analyzed by gas chromatography-electron capture detector/nitrogen phosphorus detector. Method consisted with acetone/acetonitrile (9 : 1) extraction and dichloromethane partition, followed by florisil cartridge purification with hexane/dichloromethane/acetonitrile (50 : 45 ; 5) elution. Among 197 pesticides (194 kinds) spiked to food materials, 143 and 155 pesticides were recovered over 70% on potatoes and carrots, respectively. Nineteen pesticides including bromacil, cyproconazole, were not detected in water and sample matrices. Matrix components may affect the low detections of 25 pesticides such as benfuracarb, bitertanol from potatoes and 16 pesticides such as bitertanol, carbosulfan from Carrots. Some pesticides including dichlobenil, fluoroimide and iprodione were highly detected from one or both matrices even though they were not detected from water.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.417-433
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• 2011

The study tested QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation and HPLC-MS/ MS analysis for measurement of pesticide residues in fruit and vegetable. 240 kinds of pesticides spiked at three levels of 90, 45, 9 ng/g in lettuce and apple. For QuEChERS sample preparation, graphitized carbon black (GCB) was used for only lettuce in dispersive-SPE as absorbent. Matrix-matched standard calibration was used for quantitative analysis of HPLC-MS/MS. 218 pesticides (91%) in apple and 207 pesticides (86%) in lettuce showed recoveries in the range of 70~120% with $RSD{\leq}20%$. The lowest calibrated level (LCL) were 4.5 ng/g for 192 pesticides, 9 ng/g for 42 pesticides, 45 ng/g for 3 pesticides and 3 pesticides were not detected at all concentration levels. The results showed that the QuEChERS sample preparation and HPLC-MS/MS analysis can be applied to multi-residue analysis of pesticides in vegetables and fruits.