• Title/Summary/Keyword: Residues

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Development of Standard Operating Procedures (SOPs), Standardization, TLC and HPTLC Fingerprinting of a Polyherbal Unani Formulation

  • Naaz, Arjumand;Viquar, Uzma;Naikodi, Mohammad Abdul Rasheed;Siddiqui, Javed Inam;Zakir, Mohammad;Kazmi, Munawwar Husain;Minhajuddin, Ahmed
    • CELLMED
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    • v.11 no.4
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    • pp.21.1-21.9
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    • 2021
  • Background: Unani System of Medicine (USM) has its origin to Greece. To ensure and develop the quality, authenticity of Unani drugs, standardization on modern analytical parameter is essential requirement for drugs. Objectives: The aimed of the present study was to develop a standard profile of "Qurṣ-e-Mafasil" by systematic study through authenticated ingredients, pharmacognostic identification followed by physicochemical, TLC, HPTLC fingerprinting analysis as per standard protocol. Material and Methods: In this study three batches of "Qurṣ-e-Mafasil" QM were prepared by standard method as per UPI had been followed by organoleptic properties of formulation such as appearance, color, odor, taste. Powder Microscopy and physicochemical studies were carried out such as Uniformity of weight, Friability, Disintegration time, hardness, LOD, ash vales and extractive values in like aqueous, alcohol & hexane. Further qualitative tests such as Thin-Layer Chromatography (TLC), and High-Performance Thin Layer Chromatography (HPTLC) studies were also carried out to develop fingerprint pattern of the alcoholic solvent extract of QM. Phytochemical screening was carried out in different solvent extracts such as alcoholic, aqueous and chloroform extracts to detect the presence phytoconstituents in the formulation QM. Heavy metals, Microbial Load Contamination and pesticidal residues were also determined. Results: Qurṣ-e-Mafasil showed tablet-like appearance, light brown colour, mild pungent odour and acrid taste. Uniformity of weight (mg), friability (rpm), and hardness (kg/cm) and disintegration time was ranged between (500 to 503), (0.0340 to 0.038), (8.40 to 8.67) and (4-5 minutes) respectively for the three batches. Loss in weight on drying at 105℃ was ranged between (8.3425 to 8.7346). Extracted values were calculated in distilled water ranged between (30.9091 to 31.4358), hexane (1.1419 to 1.4281), and alcohol (3.3352 to 3.3962). The ash values recorded were ranged between (3.7336 to 3.8378), and acid insoluble ash (0.5859 to 0.6112).

Analysis Method of Surfactants for Identification of Residue Dishwashing Detergent (세척제 잔류량 확인을 위한 계면활성제 분석법 확립)

  • Park, Na-Youn;Lee, Sojeong;Kim, Jung Hoan;Kho, Younglim
    • Journal of the Korean Chemical Society
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    • v.65 no.6
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    • pp.433-440
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    • 2021
  • Surfactants are organic compounds that have both hydrophilic and non-polar parts in one molecule, classified as non-ion, anion, cation, and amphoteric surfactants according to the charge of hydrophilic parts in aqueous state. A trace amounts may remain when vegetables and fruits are washed using type1 detergent (Vegetable and fruit detergent), and there is a possibility of exposure to the human body through ingestion. This study developed the simultaneous analysis method for 5 surfactants with LC-MS/MS for analysis of detergent residues after washing vegetables and fruits with detergent. The mobile phase used distilled water and acetonitrile containing 50 mM ammonium formate and 0.1% formic acid and was analyzed using a gradient method using XBridge BEH C8 column. The accuracy of the established method was 83.9-112.1%, and the precision was less than 20%. The detection limit was 7.0 (SLS) to 29.0 (SLES-N3) ㎍/L, and the correlation coefficient (r2) of calibration line regression was greater than 0.99, it is considered suitable for the analysis of trace amounts of surfactant components remaining in vegetables and fruits.

Suppression of a Residue 173 Mutant Form on Aggregation of Tryptophan Synthase α-Subunits from Escherichia coli (대장균 트립토판 중합효소 α 소단위체의 응집 형성에 미치는 잔기 173 치환체의 억제 효과)

  • Jeong, Jae Kap;Park, Hoo Hwi;Lim, Woon Ki
    • Journal of Life Science
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    • v.32 no.9
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    • pp.729-733
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    • 2022
  • Aggregation of normally soluble proteins can cause disease-related problems. Tryptophan synthase α-subunit (αTS) in E. coli adopts one of most popular structural scaffolds, the TIM barrel fold. Previous mutagenesis of the αTS gene resulted in many aggregation-prone mutant proteins. Here, Y173F (Tyr at residue 173 to Phe) substitution, which imparts increased stability, was tested for its ability to suppress aggregation of aggregation-prone mutant proteins (Y4C, S33L, P28L, P28S, G44S, D46N, P96L, and P96S). Aggregation was suppressed in all eight severe aggregate-forming mutants (all differing in their mutation positions), by the Y173F replacement. P28L αTS, which was available in pure form, was further analyzed and showed reduced secondary structure content, lower stability, and a looser structure with more exposed hydrophobic surface compared to the wild type protein. A double mutant P28L/Y173F protein showed almost no indication of these changes compared to the wild type protein. We hypothesized that Tyr at position 173 in αTS is positioned at the hydrophobic core and may serve to suppress the aggregation of this protein caused by other residues. Important residue (s) could be working widely in the prevention/suppression of protein aggregation.

Cloning and Functional Studies of Pro-Apoptotic MCL-1ES BH3M (세포사멸을 유도하는 새로운 단백질인 MCL-1ES BH3M의 클로닝 및 기능연구)

  • Kim, Jae-Hong;Park, Mira;Ha, Hye-Jeong;Lee, Kangseok;Bae, Jeehyeon
    • Development and Reproduction
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    • v.12 no.3
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    • pp.297-303
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    • 2008
  • BCL-2 family members are essential protein for the regulation of cell death and survival consisting both antiapoptotic and pro-apoptotic proteins. In the present study, we designed and cloned a new apoptotic molecule MCL-1ES BH3M coding a modified protein of MCL-1L. Compared to MCL-1L protein, MCL-1ES BH3M lacks the PEST motifs known to be involved in MCL-1L protein degradation and has seven mutated residues in BH3 domain critical for dimerization with BCL-2 family members. Overexpression of MCL-1ES BH3M induced death of different cells, and its cell killing effect was not blocked by forced expression of the pro-survival protein MCL-1L. Expression of MCL-1ES BH3M protein led to the activation of caspase 9 and caspase 3, suggesting apoptotic cell death, and confocal fluorescent microscopic analyses showed that MCL-1ES BH3M was partially localized in mitochondria. In conclusion, we reported a new apoptotic molecule and determined its cell death activity in cells.

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Column Comparison for the Separation of Ferimzone Z and E Stereoisomers and Development of Trace Residue Analysis Method in Brown Rice Using HPLC-MS/MS (컬럼 비교를 통한 Ferimzone Z 및 E 입체 이성질체의 물질 분리 및 HPLC-MS/MS를 활용한 현미 중 미량잔류분석법 개발)

  • Mun-Ju Jeong;So-Hee Kim;Hye-Ran Eun;Ye-Jin Lee;Su-Min Kim;Jae-Woon Baek;Yoon-Hee Lee;Yongho Shin
    • Korean Journal of Environmental Agriculture
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    • v.42 no.3
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    • pp.203-210
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    • 2023
  • Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C18 and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

Life Cycle Greenhouse Gas Emission Assessment on Locally Generated Kenaf Residue Biomass Fuel in South Korea (EU RED-II 방법론을 적용한 국내 미이용 바이오매스 케나프 펠릿의 전과정 온실가스 배출량 산정)

  • Youn Il Kim;Sun Young Jung;Youngjae Jo;Sung Yoon;Byung Hwan Um
    • Korean Chemical Engineering Research
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    • v.61 no.2
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    • pp.258-264
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    • 2023
  • The greenhouse gas (GHG) emission assessment of kenaf pellet, produced from locally generated kenaf residues in South Korea, has been studied based on the EU RED-II methodology for calculating GHG impact of biomass fuels. Based on the production pathway of kenaf residue pellet and emission coefficients from EU JRC report, the life cycle GHG emission of kenaf residue pellet is assessed as 3.0 gCO2eq/MJpellet and the life cycle GHG emission of electricity generated from kenaf residue pellet is assessed as 11.9 gCO2eq/MJ when electrical efficiency of final conversion is 25%. The potential GHG emission reduction of electricity produced from kenaf pellet is 90.3% compared to the domestic electricity emission factor 42.8 kgCO2eq/MWh. Also, the electricity produced from kenaf pellet can reduce at least 59.6% of GHG emission compared to the electricity produced from imported wood pellets.

Safety investigation of the moisturizing medium prepared using the Chinese oak mushroom (Lentinula edodes) based on the presence of residual pesticides, heavy metals, and radioactive materials (중국산 표고(Lentinula edodes) 보습배지의 잔류농약, 중금속 및 방사능 안전성 분석)

  • Jang, Eun-Kyoung;Jeong, Sang-Wook;Jang, Hye-Mi;Ban, Seung-Eon
    • Journal of Mushroom
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    • v.20 no.1
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    • pp.22-28
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    • 2022
  • In order to provide basic data for preparing management standards and to verify the safety of the Chinese oak mushroom-derived moisturizing medium-which is synthesized and imported in large quantities-the presence of 321 residual pesticides, 7 heavy metals, and 3 radioactive materials was analyzed in the moisturizer samples. Examination of residual pesticides in seven moisturizing medium samples prepared using the Chinese oak mushroom and three domestic sawdust samples used for mushroom culture revealed the presence of cypermethrin and iprodione in three moisturizer samples, but the contents of these pesticides were below the standard limits. Zn was detected in ten samples, Cu was detected in nine samples, and Ni was detected in four samples, but their contents were below the standard limits. Pb, Cd, Cr, and Hg were not detected in any sample. No radioactive materials were detected in the samples. In addition, fruiting bodies of the oak mushroom were observed in each medium. Examination did not reveal the presence of any residual pesticides or harmful compounds. In this study, the use of the moisturizing medium prepared using the Chinese oak mushroom was found to be safe. As residual pesticides, heavy metals, and radioactivity-even in trace amounts-remain concentrated in the human body, continuous verification of the safety of hazardous substances and pollutants during the systematic cultivation and management of these mushrooms is required.

Determination of lercanidipine in human plasma by LC-MS/MS (LC-MS/MS를 이용한 혈장 중 레르카니디핀의 분석)

  • Jang, Moon-Sun;La, Sookie;Chang, Kyu Young;Kang, Seung Woo;Han, Sang Beom;Lee, Kyung Ryul;Lee, Hee Joo
    • Analytical Science and Technology
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    • v.21 no.1
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    • pp.34-40
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    • 2008
  • Liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for the quantitative determination of lercanidipine in human plasma. After addition of internal standard (amlodipine), plasma was precipitated with acetonitrile and the supernatant was evaporated. The residues were dissolved in 50 % acetonitrile and analyzed by LC-MS/MS. Using MS/MS with multiple reaction monitoring(MRM) mode, lercanindipine were selectively detected without severe interference from human plasma. The standard calibration curve for lercanidipine was linear (r = 0.9994) over the concentration range 0.05-20.0 ng/mL in human plasma. The intra- and inter-day precision over the concentration range of lercanidipine was lower than 11.7 % (correlation of variance, CV), and accuracy was between 94.4-114.8 %. This method has been successfully applied to the pharmacokinetic study of lercanidipine in human plasma.

Determination of residual novobiocin in livestock products and fisheries products by HPLC (HPLC를 이용한 축·수산 식품 중 잔류 노보비오신의 분석)

  • Lee, Byung Kyu;Lee, Cheol-Woo;Lee, Sang-Ju;Jung, Eun Ha;Lim, Hyun Kyun;Han, Sang Beom
    • Analytical Science and Technology
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    • v.20 no.4
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    • pp.347-354
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    • 2007
  • A simple and rapid high-performance liquid chromatography assay for the determination of residual novobiocin levels in bovine, porcine, chicken, flatfish and japanese eel muscle has been developed and validated. The separation condition for HPLC/UV was optimized with phenyl hexyl ($4.6{\times}150mm$, $5{\mu}m$) column with 10 mM monobasic sodium phosphate buffer (pH 2.5)/acetonitrile (50/50, v/v) as the mobile phase at a flow rate of 1.0 mL/min and detection wavelength was set at 254 nm. Residues were extracted from tissue by blending with methanol and lipid materials were removed with n-hexane. Then, the methanol extract was evaporated to dryness under a nitrogen stream, reconstituted in the mobile phase. Aliquot of the organic extract was decanted and filtered through $0.45{\mu}m$ syringe filter. The $20{\mu}L$ of the resulting solution was injected into the HPLC system. The calibration ranges were $0.5{\sim}5{\mu}g/g$ and calibration curves were linear with coefficients of correlation better than 0.95. The limits of quantification were $0.5{\mu}g/g$ for all muscles. The recoveries of bovine, porcine, chicken, flatfish and japaneseel muscles were 99.8%, 102.4%, 91.0%, 104.0% and 93.0%, respectively. The procedures were validated according to the CODEX guideline, determining specificity, linearity, accuracy, precision, quantitation limit and recovery.

Simultaneous analysis of residual glucocorticoids in egg by LC/MS/MS (LC/MS/MS를 이용한 계란 중 잔류 글루코코티코이드의 동시분석)

  • Jang, Mi-Ae;Myung, Seung-Woon
    • Analytical Science and Technology
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    • v.22 no.4
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    • pp.326-335
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    • 2009
  • A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.