• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.401-416
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• 2011

The recent trend for pesticide residue analysis in food involves fast cleanup and use of mass spectrometry to achieve quantitative and qualitative analysis at the same time. Recently, the QuEChERS (quick, easy, cheap, effective, rugged and safe) multi-reside method has received much attention as a fast extraction and cleanup method of pesticide residue analysis. Therefore, multi-residue analysis of 236 pesticides was tested with the QuEChERS method by concurrent use of PTV-GC/TOFMS (gas chromatography/ time-of-flight mass spectrometry with programmable temperature vaporizer). PTV condition was optimized and when the method was applied to apples, pesticide recovery rates (spiked at 400 ng/g) ranged from 80% to 120%, and RSD values were under 10% for most compounds. The results showed that the QuEChERS sample preparation and PTV-GC/TOFMS analysis can be applied to multi-residue analysis of pesticides in fruits and vegetables.

• The Korean Journal of Pesticide Science
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• v.20 no.1
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• pp.23-29
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• 2016

This study was carried out to survey residual characteristics of pesticide in fresh ginsengs collected from 45 markets at 15 regions in Korea using multiresidue analysis with a GC-MS/MS and an LC-MS/MS. After residue analysis was performed, the pesticides detected from ginsengs were quantitated using their analytical methods validated by recovery tests with a GC-ECD/NPD. As a results of analysis of pesticide residue, cypermethrin, fenitrothion, fludioxonil, thifluzamide, and tolclofos-methyl were detected from 16 samples among 45 samples in total, indicating detection rate was 35.6%. Tolclofos-methyl was found to be highest in detection frequency in ginseng. Fenitrothion that has not established maximum residue limit and pre-harvest interval for ginseng was detected. The amounts of all pesticides detected were less than their MRLs. Ratios of estimated daily intakes to acceptable daily intakes of the detected pesticides in ginseng were found to be from 0.03 to 16.67%.

• Journal of Forest and Environmental Science
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• v.13 no.1
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• pp.134-142
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• 1997

Pectin and tannin analysis were carried out to inverstigate any available components from Pinus densiflora, P. koraiensis, P. thunbergii and P. rigida. To analyze terpenoid components, the essential oils were extracted with steam distillation method from four kinds of pine needles. The essential oil was analyzed by GC and GC-MS spectroscopy. The results were summarized as follows: Pectin content was highest in P. koraiensis with 0.40%, and tannin content was highest in P. koraiensis with 1.05. Major components of P. densiflora needles were ${\alpha}$-pinene, ${\beta}$-caryophyllene, ${\Delta}^3$-carene and phytol. ${\alpha}$-Pinene, ${\Delta}^3$-carene, ${\beta}$-caryophyllene, germacrene D, and camphene were found major components in P. koraiensis. Major components of P. thunbergii needles were ${\beta}$-pinene, ${\alpha}$-pinene, ${\beta}$-caryophyllene and germacrene D. ${\beta}$-Pinene, ${\alpha}$-piene, humulene oxide and ${\alpha}$-elemene were major components in P. rigida. Sabinene and citronellol were infrequent components in P. koraiensis, and ${\alpha}$-pinene oxide was present only in P. rigida. ${\alpha}$-Pinene, limonene, and bornylacetate well known as the main components of green air bath were found in P. densiflora and P. koraiensis.

• Korean Journal of Food Science and Technology
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• v.29 no.3
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• pp.427-431
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• 1997

A simultaneous and rapid gas chromatographic determination of organophosphorus, organo-chlorine, carbamate, and pyrethroid pesticides in polished rice was developed. The pesticides were extracted from samples with acetone by automated soxhlet apparatus and this extract was evaporated to dryness. The residue was dissolved in hexane, the solvent was applied to a Sep-Pak florisil catridge, was eluted with 50% ethyl acetate in n-hexane, and was injected to dual GC-ECD/NPD system. This simple method affords a high recovery of hydrophilic pesticides, allows rapid analysis, and is cheap to perform. Except for dichlorvos and captan, recoveries of 46 pesticides were over 60%.

• Journal of the Korea Academia-Industrial cooperation Society
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• v.15 no.7
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• pp.4682-4691
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• 2014

Banhabaekchulchhonma-tang is a traditional Korean herbal prescription with a range of pharmacological activities. In this study, the simultaneous analysis of 12 kinds of marker components, Homogentisic acid, Hesperidin, Naringin, Alisol A, Atractylenolide II, Atractylenolide III, Ginsenoside Rg1, Formononetin, Gastrodin, Berberine, Palmatine and 6-gingerol, in Banhabaekchulchhonma-tang was performed using high-performance liquid chromatography (RP-HPLC). The standard sample of commercial $C_{18}$ reversed phase-column using water (0.1% TFA) and acetonitrile as the mobile phase with a step gradient elution mode. The flow rate (1.0mL/min), injection volume ($10{\mu}L$) and column oven temperature ($40^{\circ}C$) at a 200, 220, 280 and 340nm wavelength was conducted. All calibration curves of the standard components showed good linearity ($r^2$ >0.999). In addition, the limit of detection (LOD) and limit of quantification (LOQ) ranged from 0.012 to $0.878{\mu}g/mL$ and 0.009 to $0.290{\mu}g/mL$. The precision intra-day and inter-day were ranged from 0.07 to 1.21% and 0.20 to 0.90%, respectively. The recoveries ranged from 97.17 to 108.40%. Each sample amount showed a very small change. These results highlight the efficient quality evaluation of Banhabaekchulchhonma-tang.

• Journal of Environmental Health Sciences
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• v.27 no.1
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• pp.88-92
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• 2001

The simultaneous analytical method for 37 residual pesticides was developed by a gas chromatography with $^{63}$ Ni electron capture detector. Pesticides added in soybean sample were extracted with 70% acetone in water and methylene chloride in oder, and then cleaned up via open-column apparatus packed with florisil and alumina N. The Ultra-2 fused capillary column was used to separate the products. The resolution between the last isomeric peak of cypermethrin (56.398 min) and the first isomeric peak of flucythrinate (56.421 min) was not satisfactory and the last isomeric peak of fenvalerate(58.783 min) and the first isomeric peak of fluvalinate(58.835 min) was overlapped. Except for $\alpha$-BHC, dichlofluanid, captan, and captafol, most recoveries were showed over 70%.

• Journal of Environmental Science International
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• v.12 no.10
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• pp.1117-1120
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• 2003

Pesticides were extracted from samples with 70% acetone and methylene chloride in order, and then cleaned up via open-column chromatography apparatus packed with florisil, and finally analyzed simultaneously the organophosphorus pesticides using GC/NPD. Ultra-2 and Ultra-1 fused silica capillary columns were used to separate and identify the products. Recovery of most analytes from soybean sample, taken from pesticide residues well, was greater than(80%) for all except(6) analytes. This method can simultaneously determine multiple pesticides with a high degree of accuracy and precision.

• Korean Journal of Environmental Agriculture
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• v.28 no.3
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• pp.266-273
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• 2009

This study was conducted to develop more convenient simultaneous determination method by matrix solid phase dispersion (MSPD) and HPLC for sulfonamides such as sulfamerazine (SMR), sulfamethazine (SMT), sulfamonomethoxine (SMM), sulfadimethoxine (SDM), sulfaquinoxaline (SQX), and tetracyclines including oxytetracycline (OTC), tetracycline (TC) chlortetracycline (CTC) in prok and flatfish. The limits of detection were 0.047 $mg{\cdot}kg^{-1}$ for OTC, TC, SMR, SMT and SMM, and 0.033 $mg{\cdot}kg^{-1}$ for CTC, SDM, and SQX, respectively. So it is sufficiently possible to detect the eight tetracyclines and sulfonamides under their MRLs ($0.1{\sim}0.2mg{\cdot}kg^{-1}$). The average percentage recoveries of sulfonamides and tetracyclines from pig muscle and flatfish spiked standard solution were approximately $80.25{\sim}101.25%$ and $85.77{\sim}121.42%$, respectively. Therefore this method was efficient for simultaneous analysis of eight tetracyclines and sulfonamides.

• Bulletin of Food Technology
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• v.21 no.2
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• pp.49-54
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• 2008

농산물 중 잔류농약을 보다 쉽고 효율적으로 분석 할 수 있는 다성분 동시분석 방법에 따라서 UPLC-PDA을 이용하여 기기조건에 따른 검출한계 및 정량한계를 식품별 최저 MRL과 비교하여 유효성을 알아보고 회수율을 통하여 방법의 재현성을 조사한 결과 다음과 같다. 41종의 농약에 대한 검량선은 직선성이 우수하였으며 검출한계 $0.005{\sim}0.109mg/kg$으로 나타났으며 정량한계 는 $0.018{\sim}0.363ppm$으로 나타났다. Cycloprothrin 등의 경우처럼 검출기의 감응도가 최저 MRL 기준을 초과하는 농약에 대한 보완으로는 검출감도가보다 우수한 UV 검출기 등의 병행 활용이 필요하다. 회수율에 따른 재현성은 쌀의 경우 첨가 농도 0.4 mg/kg 일때 $62.09{\sim}99.58%$로 편차범위는 $1.03{\sim}13.92%$ 얻을 수 있었다.

• Korean Journal of Environmental Agriculture
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• v.31 no.2
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• pp.157-163
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• 2012

BACKGROUND: For the safety of imported agricultural products, the study was conducted to develop the analytical method of unregistered pesticides in domestic. The analytical method of 6 pesticides, chlorthal-dimethyl, clomeprop, diflufenican, hexachlorobenzene, picolinafen, and propyzamide, for a fast multi-residue analysis were established for two different type crops, orange and brown rice by GC-ECD and confirmed by mass spectrometry. METHODS AND RESULTS: The analytical method was evaluated to limit of quantification, linearity and recoveries. The crop samples were extracted with acetonitrile and performed cleanup by liquid-liquid partition and Florisil SPE to remove co-extracted matrix. The extracted samples were analyzed by GC-ECD with good sensitivity and selectivity of the method. The limits of quantification (LOQ) range of the method with S/N ratio of 10 was 0.02~0.05 mg/kg for orange and brown rice. The linearity for targeted pesticides were $R^2$ >0.999 at the levels ranged from 0.05 to 10.0 mg/kg. The average recoveries ranged from 74.4% to 110.3% with the percentage of coefficient variation in the range 0.2~8.8% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in brown rice. And the average recoveries ranged from 77.8% to 118.4% with the percentage of coefficient variation in the range 0.2~6.6% at two different spiking levels (0.02 mg/kg and 0.2 mg/kg, 0.05 mg/kg and 0.5 mg/kg) in orange. Final determination was by gas chromatography/mass spectrometry/selected ion monitoring (GC/MS/SIM) to identify the targeted pesticides. CONCLUSION: As a result, this developed analytical method can be used as an official method for imported agricultural products.