• Title/Summary/Keyword: quantitation

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Development of Simultaneous Analysis for Multiple Agricultural Pesticides in Raw Milk Products using GC-MS/MS (GC-MS/MS를 이용한 원유 원료 중 농약 동시분석법 확립)

  • Young Nae Choi;Yoon ho Shin;Hwangeui Cho;Jung Bok Kim
    • Journal of Food Hygiene and Safety
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    • v.38 no.6
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    • pp.420-429
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    • 2023
  • GC-MS/MS using liquid-liquid extraction (LLE) and C18 cartridges was used to identify and quantify levels of chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin and permethrin in bulk raw milk. A calibration curve spanning 10 ng/mL to 200 ng/mL was obtained with a satisfactory correlation coefficient of 0.99. The limits of detection (LOD) and limits of quantitation (LOQ) for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in the matrix ranged from 0.06 to 1.81 ng/mL and 0.19 to 6.04 ng/mL, respectively. The recoveries of 5 pesticides from spiked samples at 37.5-125 ng/mL ranged from 86.1 to 102.1%. The measurement of uncertainty of the GC-MS/MS method for these five pesticides was developed based on the analytical process and quantification. An analysis method that is easier and faster than the method specified in the Korean food standards codes for analyzing these five pesticides in raw material milk was developed. Moreover, the analytical method for chlorpyrifos, chlorpyrifos-methyl, cypermethrin, deltamethrin, and permethrin in bulk raw milk by GC-MS/MS was established.

Wedelolactone Promotes the Chondrogenic Differentiation of Mesenchymal Stem Cells by Suppressing EZH2

  • Wei Qin;Lin Yang;Xiaotong Chen;Shanyu Ye;Aijun Liu;Dongfeng Chen;Kunhua Hu
    • International Journal of Stem Cells
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    • v.16 no.3
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    • pp.326-341
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    • 2023
  • Background and Objectives: Osteoarthritis (OA) is a degenerative disease that leads to the progressive destruction of articular cartilage. Current clinical therapeutic strategies are moderately effective at relieving OA-associated pain but cannot induce chondrocyte differentiation or achieve cartilage regeneration. We investigated the ability of wedelolactone, a biologically active natural product that occurs in Eclipta alba (false daisy), to promote chondrogenic differentiation. Methods and Results: Real-time reverse transcription-polymerase chain reaction, immunohistochemical staining, and immunofluorescence staining assays were used to evaluate the effects of wedelolactone on the chondrogenic differentiation of mesenchymal stem cells (MSCs). RNA sequencing, microRNA (miRNA) sequencing, and isobaric tags for relative and absolute quantitation analyses were performed to explore the mechanism by which wedelolactone promotes the chondrogenic differentiation of MSCs. We found that wedelolactone facilitates the chondrogenic differentiation of human induced pluripotent stem cell-derived MSCs and rat bone-marrow MSCs. Moreover, the forkhead box O (FOXO) signaling pathway was upregulated by wedelolactone during chondrogenic differentiation, and a FOXO1 inhibitor attenuated the effect of wedelolactone on chondrocyte differentiation. We determined that wedelolactone reduces enhancer of zeste homolog 2 (EZH2)-mediated histone H3 lysine 27 trimethylation of the promoter region of FOXO1 to upregulate its transcription. Additionally, we found that wedelolactone represses miR-1271-5p expression, and that miR-1271-5p post-transcriptionally suppresses the expression of FOXO1 that is dependent on the binding of miR-1271-5p to the FOXO1 3'-untranscribed region. Conclusions: These results indicate that wedelolactone suppresses the activity of EZH2 to facilitate the chondrogenic differentiation of MSCs by activating the FOXO1 signaling pathway. Wedelolactone may therefore improve cartilage regeneration in diseases characterized by inflammatory tissue destruction, such as OA.

Residual Characteristics and Processing Factors of Difenoconazole in Fresh Ginseng and Processed Ginseng Products (인삼 및 가공품 중 difenoconazole의 잔류특성 및 가공계수)

  • Noh, Hyun-Ho;Lee, Kwang-Hun;Lee, Jae-Yun;Lee, Eun-Young;Park, Young-Soon;Park, Hyo-Kyoung;Oh, Jae-Ho;Im, Moo-Hyeog;Lee, Yong-Jae;Baeg, In-Ho;Kyung, Kee-Sung
    • The Korean Journal of Pesticide Science
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    • v.16 no.1
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    • pp.35-42
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    • 2012
  • This study was carried out to elucidate the residual characteristics and calculate processing factors of difenoconazole in ginseng and its processed products, such as dried ginseng, red ginseng and their water and alcohol extracts. The pesticide was sprayed onto the ginseng according to its pre-harvest intervals in 2009 (four-year-old ginseng) and 2010 (five-year-old ginseng). Harvested ginseng was processed to dried ginseng, red ginseng and their extracts according to the commercially well-qualified conventional methods provided by the Korea Ginseng Corporation. Limit of detection (LOD) and limit of quantitation (LOQ) of difenoconazole in fresh ginseng were 0.001 and 0.003 mg/kg, respectively. In case of processed ginseng products, their levels were 0.002 and 0.007 mg/kg, respectively. Concentration of difenoconazole in both fresh ginseng and its processed products increased with the experimental period. Processing factors, calculated as a ratio of difenoconazole concentration in processed products to fresh ginseng were found to be 1.71 to 2.17 and 1.62 to 2.03 in case of dried and red ginseng, respectively, while those for their extracts ranged from 1.76 to 2.98. In case of five-year-old dried ginseng and red ginseng as well as their extracts, the ranges of processing factor of difenoconazole were found to be 2.9 to 3.1, 1.9 to 2.2 and 2.4 to 4.7, respectively.

Establishment of an Analytical Method for Prometryn Residues in Clam Using GC-MS (GC-MS를 이용한 바지락 중 prometryn 잔류분석법 확립)

  • Chae, Young-Sik;Cho, Yoon-Jae;Jang, Kyung-Joo;Kim, Jae-Young;Lee, Sang-Mok;Chang, Moon-Ik
    • Korean Journal of Food Science and Technology
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    • v.45 no.5
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    • pp.531-536
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    • 2013
  • We developed a simple, sensitive, and specific analytical method for prometryn using gas chromatography-mass spectrometry (GC-MS). Prometryn is a selective herbicide used for the control of annual grasses and broadleaf weeds in cotton and celery crops. On the basis of high specificity, sensitivity, and reproducibility, combined with simple analytical operation, we propose that our newly developed method is suitable for use as a Ministry of Food and Drug Safety (MFDS, Korea) official method in the routine analysis of individual pesticide residues. Further, the method is applicable in clams. The separation condition for GC-MS was optimized by using a DB-5MS capillary column ($30m{\times}0.25mm$, 0.25 ${\mu}m$) with helium as the carrier gas, at a flow rate of 0.9 mL/min. We achieved high linearity over the concentration range 0.02-0.5 mg/L (correlation coefficient, $r^2$ >0.998). Our method is specific and sensitive, and has a quantitation limit of 0.04 mg/kg. The average recovery in clams ranged from 84.0% to 98.0%. The reproducibility of measurements expressed as the coefficient of variation (CV%) ranged from 3.0% to 7.1%. Our analytical procedure showed high accuracy and acceptable sensitivity regarding the analytical requirements for prometryn in fishery products. Finally, we successfully applied our method to the determination of residue levels in fishery products, and showed that none of the analyzed samples contained detectable amounts of residues.

Fermentable Sugar Contents of Commercial Medical Foods and Carbohydrate Ingredients (상업용 메디컬푸드 및 탄수화물 급원의 발효성 당류 함량에 관한 연구)

  • Shin, Hee-Chang;Kang, Nam-Hee;Lee, Jang-Woon;Lee, Yoon-Bok;Lee, Kyun-Hee;Oh, Seung-Hyun
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.44 no.8
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    • pp.1200-1205
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    • 2015
  • Medical foods are enteral nutrition for patients, but they cause maladaptation symptoms like diarrhea. Although the cause of diarrhea remains unknown, some studies have indicated that the cause of diarrhea is fermentable oligosaccharides, disaccharides, monosaccharides, and polyols (FODMAP). This is a consideration for medical foods since they are easily fermented by intestinal bacterial. In this study, we estimated the FODMAP contents of commercial medical foods and carbohydrate ingredients. We measured the concentrations of FODMAP in 13 types of different medical foods and five types of carbohydrate ingredients by using high performance liquid chromatography with an evaporative light scattering detector (HPLC-ELSD). The limits of detection of FODMAP were fructose, 0.002; lactose, 0.010; raffinose, 0.003; stachyose, 0.032; 1-kestose, 0.005; nystose, 0.012; and 1-fructofuranosylnystose, 0.003 mg/kg. Limits of quantitation of FODMAP were fructose, 0.008; lactose, 0.033; raffinose, 0.009; stachyose, 0.107; 1-kestose, 0.015; nystose, 0.042; and 1-fructofuranosylnystose, 0.011 mg/kg, respectively. Concentration of FODMAP ranged from 0.428~2.968 g/200 mL. Concentrations of carbohydrate ingredients in FODMAP were chicory fiber, 278.423; soy fiber, 27.467; indigestible maltodextrin, 52.384; maltodextrin (DE10~15), 32.973; and maltodextrin (DE15~20), 50.043 g/kg. Contents of carbohydrates were 19.0~41.0 g/200 mL in commercial medical foods. We expected a correlation between contents of carbohydrates and FODMAP, as carbohydrates included FODMAP. However, we detected a low correlation (r=0.55). Since most commercial medical foods have a similar carbohydrate ingredients and nutritional values, the difference between products was determined by FODMAP contents of carbohydrate ingredients. In this study, we analyzed FODMAP contents of commercial medical foods and carbohydrate ingredients. These results are expected to be utilized as basic data for product development and minimizing maladaptation of medical foods.

Antioxidant activities and Validation of Analytical Method of Marker compounds in strawberry fruits from various cultivars (딸기 품종별 추출물의 항산화활성 및 지표성분 밸리데이션)

  • Yong, Ye Seul;Lee, Songmi;Byun, Na-Young;Sun, Sangouk;Kim, Min-Jung;Jang, Seo Woo;Jang, Won Suk;Lee, Sun Yi;Yim, Soon-Ho
    • Korean Journal of Food Science and Technology
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    • v.51 no.6
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    • pp.517-523
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    • 2019
  • In this study, we investigated antioxidant capacity of 20 strawberry extract using the DPPH and ABTS assay and HPLC-DAD validation method. The total polyphenolic and flavonoids contents of 20 strawberry extracts were 22.77-107.61 mg TAE/100 g FW and 17.58-44.12 mg QE/100 g FW. The Aiberry and Elie star showed the highest total polyphenol and flavonoid contents, respectively. The DPPH radical scavenging activity of what was 1540.6-1124.0 μmol TEAC/100 g FW and Derunoka showed the highest activity. The ABTS radical scavenging activity was 6352.3-4592.3 μmol TEAC/100 g FW and FA23 showed the highest activity. The HPLC-DAD method for the quantitation of ellagic acid results showed high linearity in various concentration ranges, and the limit of detection was 2.35 μg/mL. The limit of quantification was 7.12 μg/mL. Relative standard deviation values from intra-and inter-day precision were less than 5.31%. Recovery rate at 10, 50, and 100 μg/mL, respectively, were 100.0-101.0% with relative standard deviation (RSD) values less than 5.30%. These results provide viable information for the validation of antioxidant capacity in strawberry fruits.

Simultaneous Pesticide Analysis Method for Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor and Trifluralin Residues in Agricultural Commodities Using GC-ECD/MS (GC-ECD/MS를 이용한 농산물 중 Bifenox, Ethalfluralin, Metolachlor, Oxyfluorfen, Pretilachlor, Thenylchlor 및 Trifluralin의 동시 분석)

  • Ahn, Kyung Geun;Kim, Gi Ppeum;Hwang, Young Sun;Kang, In Kyu;Lee, Young Deuk;Choung, Myoung Gun
    • Korean Journal of Environmental Agriculture
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    • v.37 no.2
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    • pp.104-116
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    • 2018
  • BACKGROUND: This experiment was conducted to establish a simultaneous analysis method for 7 kinds of herbicides in 3 different classes having similar physicochemical property as diphenyl ether(bifenox and oxyfluorfen), dinitroaniline (ethalfluralin and trifluralin), and chloroacetamide (metolachlor, pretilachlor, and thenylchlor) in crops using GC-ECD/MS. METHODS AND RESULTS: All the 7 pesticide residues were extracted with acetone from representative samples of five raw products which comprised apple, green pepper, Kimchi cabbage, hulled rice and soybean. The extract was diluted with saline water and directly partitioned into n-hexane/dichloromethane(80/20, v/v) to remove polar co-extractives in the aqueous phase. For the hulled rice and soybean samples, n-hexane/acetonitrile partition was additionally employed to remove non-polar lipids. The extract was finally purified by optimized Florisil column chromatography. The analytes were separated and quantitated by GLC with ECD using a DB-1 capillary column. Accuracy and precision of the proposed method was validated by the recovery experiment on every crop samples fortified with bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin at 3 concentration levels per crop in each triplication. CONCLUSION: Mean recoveries of the 7 pesticide residues ranged from 75.7 to 114.8% in five representative agricultural commodities. The coefficients of variation were all less than 10%, irrespective of sample types and fortification levels. Limit of quantitation (LOQ) of the analytes were 0.004 (etahlfluralin and trifluralin), 0.008 (metolachlor and pretilachlor), 0.006 (thenylchlor), 0.002 (oxyfluorfen), and 0.02 (bifenox) mg/kg as verified by the recovery experiment. A confirmatory technique using GC/MS with selected-ion monitoring was also provided to clearly identify the suspected residues. Therefore, this analytical method was reproducible and sensitive enough to determine the residues of bifenox, ethalfluralin, metolachlor, oxyfluorfen, pretilachlor, thenylchlor, and trifluralin in agricultural commodities.

Optimization of Analytical Methods for Octacosanol in Related Health-functional Foods with GC-MS (GC-MS를 이용한 건강기능식품 중 옥타코사놀 분석법 개발 연구)

  • Lee, Jin Hee;Oh, Mi Hyune;Lee, Kyung Jin;Kim, Yang Sun;Keum, Eun Hee;Park, Ji Eun;Cho, Mee Hyun;Seong, Min Hye;Kim, Sang A;Kim, Mee hye
    • Journal of Food Hygiene and Safety
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    • v.33 no.4
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    • pp.266-271
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    • 2018
  • The Ministry of Food and Drug Safety (MFDS) is amending its test methods for health-functional foods (dietary food supplements) to establish regulatory standards and specifications in Korea. In this regard, we continue our research on developing analytical methods for the items. Octacosanol is the major component of polycosanol and is a high-molecular-mass primary fatty alcohol, obtained from sugar cane wax. Previous researchers have shown that octacosanol can lower cholesterol and has antiaggregatory properties, cytoprotective uses, and ergogenic properties for human health. Recently, octacosanol products have been actively introduced into the domestic market because of their functional biological activity. We have developed a sensitive and selective test method for octacosanol that the TMS derivatives by means of gas-chromatographic-tandem mass spectrometry (GC-MS). The trimethylsilyl ether derivative of the target analyte showed excellent chromatographic properties. The procedure was validated in the range of $12.5{\sim}200{\mu}g/L$. Standard calibration curves presented linearity with the correlation coefficient ($r^2$) > 0.999, and the limits of detection (LOD) and limits of quantitation (LOQ) were $4.5{\mu}g/L$ and $13.8{\mu}g/L$, respectively. The high recoveries (92.5 to 108.8%) and precision (1.8 to 2.4%) obtained are in accordance with the established validation criteria. Our research can provide scientific evidence to amend the octacosanol test method for the Health-Functional Food Code.

Total Folate Contents of 15 Edible Plants Consumed in Korea Using Trienzyme Extraction Method (국내 소비되는 봄나물의 Trienzyme 추출법을 적용한 엽산 함량 분석)

  • Kim, Bo Min;Kim, So-Min;Oh, Ji Yeon;Cho, Young-Sook;Kim, Se-Na;Choi, Youngmin
    • Journal of the Korean Society of Food Science and Nutrition
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    • v.43 no.11
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    • pp.1796-1800
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    • 2014
  • Trienzyme digestion (AOAC Official Method 2004.05) procedure using protease, ${\alpha}$-amylase, and chicken pancreas conjugase was evaluated to determine its usefulness in the microbiological quantitation of total folate in foods. Folate values obtained by alkali hydrolysis (Korean Food Standards Codex) were compared to those obtained by the trienzyme method for four certified reference materials (CRM) representing diverse matrixes. Trienzyme treatment increased measurable folate from most CRM compared to levels found after alkali hydrolysis. The largest increases were observed with CRM 487 (pig liver, 5.8-fold) and CRM 121 (whole meal flour, 3.1-fold) after trienzyme digestion. Using trienzyme digestion method, total folate contents of raw and blanched edible plants were determined. Eleutherococcus senticosus ($146.9{\mu}g/100g$) showed the highest total folate content, followed by Aster glehni F. Schmidt ($142.8{\mu}g/100g$) and Ledebouriella seseloides H. Wolff ($140.4{\mu}g/100g$) on a wet weight basis. Blanching of samples resulted in an insignificant decrease in folate content for five samples and 11~63% reduction for nine samples. Our finding suggests that trienzyme digestion method is accurate for the determination of food folate in leafy vegetables.

Residual Change of Deltamethrin in Stream Water after Spaying for Pest Control of Stream Levee (하천둔치에 방역용 Deltamethrin 살포 시 하천수 중 잔류변화)

  • Han, Ye-Hun;Park, Jae-Hun;Lim, Jong-Sung;Lee, Yong-Ju;Lee, Sung-Kyu;Lee, Kyu-Seung
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.78-83
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    • 2013
  • BACKGROUND: This study was performed to investigate the change of deltamethrin residue after spraying for control of hygienic insects in bush of levee at Bansuk-dong stream (A) and Juk-dong ditch (B) in Yuseong, Daejeon. The drop concentrations and disappearance of deltamethrin residue in stream water were determined to evaluate the toxic effects of stream ecosystem. METHODS AND RESULTS: Water samples were collected at 7 points including 0, 5, 10, 20, 40, 70 and 100 m downstream from the deltamethrin spraying point. Water sample was partitioned into dichloromethane, and was determined with GC/${\mu}$-ECD. Limit of Quantitation of deltamethrin was 0.04 ${\mu}g/L$. Recoveries of deltamethrin at two fortification levels of 0.4 and 2.0 ${\mu}g/L$ were $91.57{\pm}3.13%$(n=3) and $94.40{\pm}4.59%$(n=3) in A stream, and $88.24{\pm}3.33%$(n=3) and $85.20{\pm}3.73%$(n=3) in B stream, respectively. Residue of A stream were from <0.04 ${\mu}g/L$ to 0.48 ${\mu}g/L$ and B stream were from 0.08 ${\mu}g/L$ to 14.95 ${\mu}g/L$ under practice application condition. And residues were from <0.04 ${\mu}g/L$ to 0.2 ${\mu}g/L$ in A stream treated deltamethrin with 1.0 mg level at the upper region. CONCLUSION(S): Practice application of deltamethrin for the pest control of waterside was not much shown toxic effect to ecosystem of stream.