• Title/Summary/Keyword: HPLC/UVD

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Method Development and Validation for Analysis of Isopyrazam Residues in Agricultural Products (농산물 중 살균제 Isopyrazam의 개별 잔류분석법 확립)

  • Kim, Ji-Yoon;Kim, Ja-Young;Ham, Hun-Ju;Do, Jung-Ah;Oh, Jae-Ho;Lee, Young-Deuk;Hur, Jang-Hyun
    • The Korean Journal of Pesticide Science
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    • v.17 no.2
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    • pp.84-93
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    • 2013
  • Validated analytical methods for isopyrazam are meager or lacking. In the present study, a single residual analytical method was developed for isopyrazam in selected commodities. Isopyrazam was analyzed in brown rice, soybean, green pepper, mandarin, cucumber, and Korean melon. We tried different solvents and methods through extraction, partition and purification steps to obtain best analytical results. For isopyrazam samples were extracted with acetonitrile, concentrated and partitioned with n-hexane, clean-up using florisil with n-hexane/ethylacetate (70/30) and analyzed with HPLC/UVD. The limit of quantitation (LOQ) for isopyrazam was 1.0 ng (S/N > 10) and method LOQ (MLOQ) was 0.04 mg $kg^{-1}$. Recovery ranged through 81.0~105.3% (syn-isomer) and 80.8~105.6% (anti-isomer) at fortification level of 0.04 (MLOQ), 0.4 (10 ${\times}$ MLOQ), and 2.0 (50 ${\times}$ MLOQ). The coefficient of variation (CV) for isopyrazam was less than 10% regardless of sample types. These results were further confirmed with LC/MS, respectively. The proposed method is highly reproducible and sensitive and is suitable for routine analysis.

Establishment of Pre-Harvest Residue Limits (PHRL) of Flubendiamide and Pyriofenone on Strawberry (Fragaria ananassa Duch.) (생산단계 잔류허용기준설정을 위한 Flubendiamide 및 Pyriofenone의 딸기(Fragaria ananassa Duch.) 중 경시적 잔류특성 연구)

  • Kim, Hee-Gon;Kim, Ji-Yoon;Hur, Kyung-Jin;Kwon, Chan-Hyeok;Hur, Jang Hyun
    • The Korean Journal of Pesticide Science
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    • v.21 no.1
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    • pp.62-67
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    • 2017
  • In this study, the residue patterns of flubendiamide and pyriofenone registered in the strawberry were investigated to predict pre-harvest residue limit (PHRL). The samples were harvested at 0, 1, 2, 3, 5, 7, 10 days after treatment and the pesticide residues were analyzed by HPLC/UVD. The limit of quantification (LOQ) was $0.01mg\;kg^{-1}$ for flubendiamide and pyriofenone. The recovery levels of flubendiamide and pyriofenone were $90.9{\pm}2.2%$ and $81.9{\pm}0.8%$, $87.7{\pm}2.1%$ and $85.3{\pm}1.1%$ for spiked levels of 0.01 and $0.1mg\;kg^{-1}$, respectively. The values of biological half-lives for field 1 and field 2 were 8.1 and 7.2 days for flubendiamide, 7.0 and 6.9 days for pyriofenone. According to these results, we recommends the level of PHRL on strawberry for flubendiamide and pyriofenone as 1.87 and $3.76mg\;kg^{-1}$ at 10 days before harvest, respectively.

Gas Chromatographic Analysis of TDI, MDI and HDI Using 2-Chlorobenzyl Alcohol and 2,4-Dichlorobenzyl Alcohol Derivatives (2-클로로벤질 알코올 및 2,4-디클로로벤질 알코올 유도체를 이용한 TDI, MDI 및 HDI의 가스크로마토그래피 분석)

  • Yun, Ju-Song;Park, Jun-Ho;Lee, Kang-Myoung;Choi, Hong-Soon;Cho, Young-Bong;Koh, Sang-Baek;Cha, Bong-Suk
    • Journal of Korean Society of Occupational and Environmental Hygiene
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    • v.16 no.3
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    • pp.222-232
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    • 2006
  • Objectives: The objective of this study was to propose the total isocyanate analytical method which involves derivation of 2,4-toluene diisocyanate(2,4-TDI), 2,6-toluene diisocyanate(2,6-TDI), 4,4'-methylenediphenyl diisocyanate(4,4'-MDI) and 1,6-hexamethylene diisocyanate(1,6-HDI) using 2-chlorobenzyl alcohol(2-CBA) or 2,4-dichlorobenzyl alcohol(2,4-DCBA), and analyzing of hydrolysate of the synthesized urethane with the gas chromatography(GC)/flame ionization detector(FID), GC/pulsed discharge ionization detector-electron capture detector(PD-ECD) and GC/mass selective detector(MSD). Methods: Urethanes were synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI to 2-CBA or 2,4-DCBA. Urethanes was verified by TLC, HPLC/UVD and GC/MSD. For field application, the most suitable condition that 2-CBA coated in glass fiber filter removed completely and urethanes were not removed was searched. 2-CBA generated from hydrolysis of urethanes according to hydrolysis conditions. Diisocyanates were collected on field air and analyzed. Results: Urethanes which were white and solid phase synthesized by reacting 2,4-TDI, 2,6-TDI, 4,4'-MDI, 1,6-HDI and 2-CBA or 2,4-DCBA. And urethanes were verified by TLC, HPLC/UVD and GC/MSD. The most suitable conditions to remove 2-CBA coated in glass fiber filter were $87^{\circ}C$ and 20 mmHg and urethanes were not removed under same condition. Hydrolysis yields of urethanes were 99 % to 111 %. 2-CBA, the hydrolysate of urethanes was analyzed by GC/FID, GC/PD-ECD and GC/MSD. Conclusions: Simultaneous analysis of 2,4-TDI, 2,6-TDI, 4,4'-MDI and 1,6-HDI deriving with 2-CBA and 2,4-DCBA, along with a total isocyanate analysis, was feasible with GC/FID, GC/PD-ECD and GC/MSD. This result will be a guide of further study on total isocyanate analysis.

Residual Characteristics of Insecticide Dinotefuran in Asparagus under Greenhouse Condition (시설재배 아스파라거스 중 살충제 dinotefuran의 잔류특성)

  • Boo, Kyung Hwan
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.19 no.6
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    • pp.375-381
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    • 2018
  • This study was performed to investigate the residual characteristics of the insecticide dinotefuran in asparagus under greenhouse conditions from July to August and consequentially to obtain basic data for guidelines on the safe use of this pesticide in asparagus. Residues of dinotefuran in young stem of asparagus before and after growing mother stem were analyzed from samples collected at 0, 1, 3, 5, and 7 days after single application of a commercial formulation of dinotefuran (wettable powder, 10%) at the recommended dose (2,000 times dilution). The residue of dinotefuran in young stem of asparagus was analyzed by HPLC-UVD, and recovery of dinotefuran in young stem was tested at 0.5 and 1.0 mg/kg concentrations. As a result, the limit of quantitation (LOQ) of dinotefuran was 0.01 mg/kg, and the recovery of dinotefuran was in the range of 83.3-94.0% with a coefficient of variation less than 10%. Residues of dinotefuran in young stem of asparagus before and after growing the mother stem were lower than the tentative limit (0.05 mg/kg) from 5 and 3 days after single application, respectively. Based on these results, single application of dinotefuran (wettable powder, 10%) at the recommended dose at 7 days before harvest would have no deleterious effects on safety issues concerning pesticide residue. This result might provide basic information to construct guidelines for the safe use of dinotefuran in asparagus.

Simultaneous Analysis of Four Standards of The Herbal Formula, DF-02, of Ephedra intermedia and Rheum palmatum, using by High Performance Liquid Chromatography-Ultraviolet Detector (HPLC-UVD)

  • Choi, Seong Yeon;Jeong, Birang;Jang, Hyeon Seok;Lee, Jiho;Kwon, Yong Soo;Yoon, Yoosik;Shin, Soon Shik;Yang, Heejung
    • Natural Product Sciences
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    • v.25 no.2
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    • pp.111-114
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    • 2019
  • The herbal formula, DF-02, consisting of Ephedra intermedia and Rheum palmatum are used for the treatment of the metabolic diseases such as obesity and liver fibrosis in Korean local clinics. We aimed to develop the simultaneous analytical conditions for four standards, (+)-pseudoephedrine (PSEP) and (-)-ephedrine (EP) for E. intermedia, and aloe-emodin (AE) and chrysophanol (CP) for R. palmatum using HPLC-UV techniques. The validated conditions yielded the high precision (relative standard deviation (RSD) < 3.65%) and the recoveries (94 - 106%) using the calibration curves with high linearity ($R^2$ > 0.9994). As a result, four standards of DF-02 were simultaneously determined under the developed method, which will be utilized for the quality control or evaluation of DF-02 and many herbal preparations containing E. intermedia and R. palmatum.

Simultaneous Determination of Sulfonamides in Porcine and Chicken Muscle Using High Performance Liquid Chromatography with Ultraviolet Detector

  • Shim, You-Sin;Shin, Dong-Bin;Cho, Yong-Sun;Choi, Yun-Hee;Lee, Sang-Hee
    • Food Science and Biotechnology
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    • v.18 no.6
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    • pp.1430-1434
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    • 2009
  • The present study used the liquid extraction pretreatment method and developed a liquid chromatographyultraviolet detector (LC-UV) for the simultaneous determination of 14 sulfonamides (SAs) residues in porcine and chicken muscle. Linearity within a range of $50-150\;{\mu}g/kg$ was obtained with the correlation coefficient ($r^2$) of 0.9673-0.9997. The mean recovery of SAs was 55.9-109.7% (relative standard deviations; RSDs 1.7-17.3%) in porcine muscle and 52.8-112.4% (RSDs 2.3-16.9%) in chicken muscle. The limits of detection (LODs) and limits of quantification (LOQs) were 2-32 and $7-96\;{\mu}g/kg$ in porcine muscle, and 4-32 and $13-97\;{\mu}g/kg$ in chicken muscle, respectively. These values were lower than the maximum residue limits (MRLs) established by the European Union. The sum of all SAs residues present should be less than $100\;{\mu}g/kg$.

A Comparison of Sampling and Analytical Methods for Airborne Isocyanates (공기중 이소시아네이트류의 측정 및 분석방법에 관한 비교연구)

  • 변혜정;윤충식;백남원
    • Journal of Environmental Health Sciences
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    • v.22 no.2
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    • pp.32-42
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    • 1996
  • This study was performed to evaluate accuracy and precision of filter method and impinger method for analyzin airborne isocyanates in mixture (2, 6-TDI, HDI, 2, 4-TDI, MDI). Filter method was performed using the OSHA Method 42 and impinger method using the NIOSH Method 5521. The samples were analyzed by high performance liquid chromatography-ultraviolet detector (HPLC-UVD). After the optimum operating conditions for each method were investigated, samples with various concentration levels were quantified at the conditions. The precision was expressed by the pooled coefficient of variation(C.V.) and the accuracy by overall accuracy. The results are summarized as follows: 1. The optimum condition of filter method was determined at 35/65 ACN/buffer (0.01 M ammonium acetate) in mobile phase. And in case of impinger method, it was at 30/70 ACN/buffer(0.2 M sodium acetate). The effect of concentrations of acetate on the separation of the peaks was not significant, but, the effect of ACN/buffer ratio was significant. 2. The correlation coefficients for the two methods were above 0.9 in all isocyanate compounds. Average recovery efficiencies for 2, 6-TDI, HDI, 2, 4-TDI and MDI in filter method were 92.4%, 102.6%, 87.3% and 101.0%, respectively. Those in impinger method were 106.6%, 106.7%, 99.0% and 103.6%, respectively. As a result, the recovery efficiency of impinger method was higher than those of filter method in analyzing isocyanate compounds. 3. The pooled coefficients of variations of the methods were slightly higher than expected. The overall accuracies of the methods were within $\pm 25%$ for each isocyanate compound. Since these results satisfy NIOSH criteria, the accuracy of the experiment is appropriate. 4. As seen above, impinger method is more efficient than filter method. But, there are many disadvantages in impinger method. Therefore, solid sorbent such as a glass fiber filter must be developed in order to have the high efficiency not less than that of impinger method in the future.

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Simultaneous Determination of Water-Soluble Vitamins (Vitamin $B_1$, $B_2$, $B_3$, $B_6$ and C) in Dietary Supplements by High-Performance Liquid Chromatography (영양보충용 식품 중 수용성비타민(Vitamin $B_1$, $B_2$, $B_3$, $B_6$ and C)의 HPLC를 이용한 동시분석법)

  • Suh, Hee-Jae;Kim, So-Hee
    • The Korean Journal of Food And Nutrition
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    • v.24 no.3
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    • pp.414-421
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    • 2011
  • 시중에 유통 중인 영양보충용 제품의 수용성 비타민 $B_1$(thiamin), $B_2$(riboflavin), $B_3$(nicotinic acid and nicotine amide), $B_6$(pyridoxine), C(ascorbic acid)의 신속한 동시분석 방법을 확립하기 위하여 본 연구를 실시하였다. 영양보충용 제품은 정제, 연질캅셀, 분말, 액상의 4가지 제형에 대해 27종의 제품을 구입한 후, Ion-pair 분리기법을 사용하여 HPLC-UVD를 이용한 동시분석 방법을 검토하였다. 비타민 $B_1$, $B_2$, $B_3$, $B_6$, C의 HPLC에 의한 동시분석 조건을 검토한 결과, 이동상은 0.02% triethylamine, 17.5% 메탄올, $5{\mu}M$ sodium hexanesulfonic acid가 함유된 pH 3.5(acetic acid로 조절)의 수용액을 사용하였고, 용출시간은 다른 피크의 영향을 받지 않도록 30분으로 하였다. 수용성 비타민의 회수율은 96% 이상이었다. 본 연구에 의해 확립된 수용성 비타민의 동시분석 조건은 검량선의 직선성, 정밀성, 정확성, 기기적합성 등이 USP 및 ICH 기준에 적합하여 HPLC의 동시분석 방법으로 합당하였다. 수용성 비타민의 추출 용매는 제형에 따라 약간의 차이를 보이긴 했으나, 물이나 산성조건을 갖춘 HPLC의 이동상이 에탄올이나 메탄올보다 높은 추출 효율을 보였다. 초음파 추출기에 의한 추출 시간은 20분이 가장 적당하였다. 본 연구의 결과는 수용성 비타민의 신속한 추출 및 분석에 매우 효율적으로 이용될 것으로 기대된다.

Changes in Reducing Sugar and Catalpol Contents of Rehmannia Root Slurry with Aging Treatments (숙성처리에 따른 지황 슬러리의 환원당 및 카탈폴 변화)

  • Jang, Gwi Yeong;Kim, Dong Hwi;Park, Chan Hum;Shin, Yu Su;Kang, Tae Su;Jeong, Heon Sang;Choi, Jehun
    • The Korean Journal of Food And Nutrition
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    • v.31 no.4
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    • pp.559-564
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    • 2018
  • Rehmannia glutinosa root (R. root) has been used as an traditional medicine, and is important resource for natural medicines and functional foods. However, R. root contains catalpol which is bitter, and undigested sugars, including stachyose and raffinose, which can cause diarrhea. Therefore, this study was performed to identify the changes in reducing sugar from undigested sugars and in catalpol contents in R. root slurry induced by aging treatments. R. root slurry was treated at $10{\sim}70^{\circ}C$ for up to 72 hr; and extracted with a 50% ethanol solution. The catalpol content was analyzed using HPLC-UVD. Reducing sugar content generated from undigested sugars was measured by the Nelson-Somogyi methods, and the reaction rates were calculated from their variation according to aging time and temperature. During the aging treatment, reducing sugar increased and catalpol decreased. Their formation and degradation rates were highest at $50^{\circ}C$ and $30{\sim}40^{\circ}C$, and their rates were $2.05mg/g{\cdot}hr$ and 23.09 to 23.33%/hr, respectively. These results indicated that aging treatment can positively affect the sweetness and digestibility of R. root slurry. Therefore, an aging treatment could be considered for improving the taste and digestibility of R. root.

Analysis of Selected Water-Soluble Vitamin B1, B2, B3, and B12 Contents in Namul (Wild Greens) Consumed in Korea (국내에서 섭취되는 나물류에 함유된 일부 수용성 비타민의 함량 분석)

  • Yoon, Jimin;Chung, Haejung;Kim, Younghwa
    • The Korean Journal of Food And Nutrition
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    • v.32 no.1
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    • pp.61-68
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    • 2019
  • In this study, the contents of water-soluble vitamins $B_1$ (thiamin), $B_2$ (riboflavin), $B_3$ (niacin), and $B_{12}$ (cyanocobalamin) in namuls (wild greens), such as salads and side dishes, consumed in Korea were quantified by high-performance liquid chromatography (HPLC) with UV and fluorescence detection. All samples were prepared with recipes used in Korea. All analyses were performed under the quality control of vitamin $B_1$, $B_2$, $B_3$, and $B_{12}$. The vitamin $B_1$, $B_2$, and $B_3$ contents in namuls consumed in Korea were analyzed. The highest content of vitamin $B_1$ was $3.018{\pm}0.016mg/100g$ in Putgochudoenjang-muchim. The highest contents of vitamin $B_2$, $B_3$, and $B_{12}$ were $0.279{\pm}0.003mg/100g$ in Gul-muchim, $12.241{\pm}0.040mg/100g$ in Chamchi-salad, and $8.133{\pm}0.371{\mu}g/100g$ in Pijogae-muchim, respectively. These results showed that animal-based ingredients in salads provided for good intake of vitamin $B_{12}$. These results can be used as basic data for food composition tables and improvement of the national health of Koreans.