MOLECULES
·
2022
·Vol. 27
·期 6
·1950
·
IF 4.927
Yue Wang,Jing Feng,Song Wu,Huihui Shao,Wenxuan Zhang,Kun Zhang,Hanyilan Zhang,Qingyun Yang
A new derivatization high-performance liquid chromatography method with ultraviolet detection was developed and validated for the quantitative analysis of methanesulfonate genotoxic impurities in an innovative drug for the treatment of non-alcoholic fatty liver disease. In this study, sodium dibenzyldithiocarbamate was used as a derivatization reagent for the first time to enhance the sensitivity of the analysis, and NaOH aqueous solution was chosen as a pH regulator to avoid the interference of the drug matrix. Several key experimental parameters of the derivatization reaction were investigated and optimized. In addition, specificity, linearity, precision, stability, and accuracy were validated. The determined results of the samples were consistent with those obtained from the derivatization gas chromatography–mass spectrometry analysis. Thus, the proposed method is a reliable and practical protocol for the determination of trace methanesulfonate genotoxic impurities in drugs containing mesylate groups.
研究领域:
药物分析
·
毒理学
·
分析化学
✓ 已验证
DOI
高影响因子
JOURNAL OF CHROMATOGRAPHY A
·
2019
·
IF 3.858
Mingxian Li,Congcong Gu,Lan Luo,Jie Zhou,Jing Liu,Feng Zheng
The selective and sensitive determination of potential genotoxic methanesulfonate impurities in drug substances is highly challenging. A new method is reported for testing of methyl methanesulfonate (MMS), ethyl methanesulfonate (EMS) and isopropyl methanesulfonate (IPMS) in active pharmaceutical ingredients (APIs). Headspace single drop microextraction (HS-SDME) with room-temperature ionic liquid (RTIL) as extractant was employed to preconcentrate analytes and eliminate the drug matrix simultaneously. In order to increase volatilities for HS extraction and to improve their reactivity of the further derivatization at the same time, sodium iodide (NaI) was added to the sample to derivatize methanesulfonates to the corresponding iodoalkanes. The iodoalkanes in the extract were derivatized with N , N -diethyldithiocarbamate (DDTC) after HS-SDME, followed by separation and detection with high-performance liquid chromatography with ultraviolet detection (HPLC-UV). Several important parameters, including reaction temperature, reaction time and concentration of NaI, sample volume, microdrop volume, stirring rate, salt addition, extraction time, concentration, reaction time and reaction temperature of DDTC were investigated. Under the optimal conditions, LODs and LOQs of all methanesulfonates were 15 ng mL −1 and 40 ng mL −1 , respectively. Linearity (correlation coefficient values r > 0.999) and precision (the relative standard deviations were 1.0–4.6%) of six repeated injections were obtained. The recoveries at three spiked concentration levels were all in the range of 86.2–107.5% with the relative standard deviations <3.5%. The method reported here avoids interference of drug substances efficiently and detects methanesulfonate impurities in high sensitivity by HPLC-UV in Imatinib Mesylate and Levofloxacin Mesylate.
研究领域:
分析化学
·
药物分析
·
毒理学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
HORTSCIENCE
·
2021
·Vol. 56
·期 8
·909-914
·
IF 1.455
Asma Mohammed Saeed Al-Kubati,Baoshan Kang,Liming Liu,Aqleem Abbas,Qinsheng Gu
Zucchini yellow mosaic virus (ZYMV) causes serious damage to cucurbit crops worldwide and can be spread by aphids, by mechanical injury, and in seeds. With the popularization of cucurbit grafting, the use of susceptible rootstock has increased the risk of ZYMV infection in cucurbit crops. In China, the bottle gourd (Lagenaria siceraria) is a widely used rootstock in grafted watermelon production. However, few resistant bottle gourds are available commercially. This study developed bottle gourd lines resistant to ZYMV using ethyl methanesulfonate (EMS) mutagenesis. A new mutated bottle gourd population (M1) was generated by treating seeds with EMS. Diverse phenotypes were observed in the seedlings, flowers, and fruit of M2 plants, some of which are of potential commercial interest, such as dwarfing and different fruit shapes. Based on the M2 phenotypes, 106 M3 lines were selected and screened for resistance to ZYMV by mechanical inoculation and agroinfiltration. Nine M3 lines were resistant to ZYMV during three tests. One inbred M4 line (177-8) was developed and showed stable resistance and no virus when tested using a double-antibody sandwich enzyme-linked immunosorbent assay (DAS-ELISA) and polymerase chain reaction. These resistant lines are promising materials for developing watermelon rootstock and exploring resistance genes as new ZYMV-resistant resources. EMS induction could be a practical strategy for creating resistant cucurbit crops.
研究领域:
植物学
·
遗传学
·
作物科学
✓ 已验证
DOI
高影响因子
ORGANIC & BIOMOLECULAR CHEMISTRY
·
2013
·Vol. 12
·期 9
·1448-1453
·
IF 3.568
Xue-Qi Zhang,Zhong-Xia Wang
Nickel-catalyzed cross-coupling of aryltrimethylammonium triflates and amines was carried out under mild conditions. The reaction has a broad scope of substrates and can be performed by a one-pot procedure from an aryldimethylamine.
研究领域:
有机化学
·
催化化学
✓ 已验证
产品关联
DOI
PubMed
高影响因子
Sustainable Materials and Technologies
·
2024
·
IF 8.6
Rui Cai,Guangjin Hu,Yujie Chenyang,Zhixing Huang,Xiaohang Wang,Benyong Han
Five new amino-acid-functionalized methanesulfonate ionic liquids ([AAH][CH 3 SO 3 ]-ILs) were prepared using methanesulfonic acid and amino acids (AAs). The catalytic performances of the five synthesized [AAH][CH 3 SO 3 ]-ILs were evaluated for biodiesel synthesis via the esterification of oleic acid with methanol. Among them, IL [GluH][CH 3 SO 3 ] exhibited the optimal catalytic activity in the oleic acid esterification. An experimental design based on the RSM-BBD was used to optimize the reaction conditions. A conversion rate of 96.8 % was attained using the [GluH][CH 3 SO 3 ] catalyst for the oleic acid esterification at a catalyst load of 12 wt%, a molar ratio of 19.6:1, a reaction time of 3.5 h and a temperature of 103 °C. The [GluH][CH 3 SO 3 ]-catalyzed oleic acid esterification followed first-order kinetics with the activation energy and frequency factor of 9.86 kJ·moL −1 and 0.47 min −1 , respectively. The catalytic activity of the [GluH][CH 3 SO 3 ] catalyst did not considerably change during ten consecutive cycles of the esterification reaction. Operational simplicity, high conversion rate along with good reusability makes the IL [GluH][CH 3 SO 3 ] a promising catalyst for replacing traditional catalysts for the biodiesel preparation via the fatty acids esterification.
研究领域:
化学工程
·
催化化学
·
能源科学
✓ 已验证
产品关联
DOI
高影响因子
Materials Chemistry Frontiers
·
2022
·Vol. 6
·期 16
·2274-2283
·
IF 8.683
Hanxiao Zhou,Tianhui Li,Wenjing Liu,Zhihao Guo,Yuxuan Guo,Jingjing Gao,Meizhen Qu,Huan Zhang,Gongchang Peng
Lithium metal is an ideal anode to replace graphite because of its high theoretical specific capacity. However, the surface of the lithium anode is prone to producing uncontrollable lithium dendrites, which seriously hinders its mass production. The morphology and chemical properties of the SEI layer have a key influence on the electrochemical precipitation of lithium ions on the electrode surface. Therefore, modifying the SEI layer is an important strategy to suppress lithium dendrites. This paper describes an effective additive, [tert-butyl(diphenyl)silyl] trifluoromethanesulfonate. The results reveal that the additive can be preferentially reduced on the surface of the lithium anode to form a flat and dense SEI layer, which further inhibits the consumption of the electrolyte and improves the electrochemical reversibility during the lithium plating/stripping process.
研究领域:
电化学
·
材料科学
·
能源存储
✓ 已验证
产品关联
DOI
高影响因子
TETRAHEDRON
·
2024
·
IF 2.1
Zixu Li,Fei Wang,Kai Ma,Chao Fang,Qiang Jia,Changhu Chu
Aryl triflate is a type of facile and readily available compounds, which could be used as an alternative substrate for Suzuki cross coupling. In this manuscript, a novel ppm-Pd-Fe/C catalyst has been developed by reduction of palladium acetate and iron trichloride with aqueous hydrazine in situ and supported on activated charcoal. In combined with Sphos, and metal zinc as additives, this catalyst, with 300 ppm palladium loading, could be applied in the Suzuki cross coupling between aryl triflates with aryl neopentylglycolboronates.
研究领域:
有机化学
·
催化
·
材料科学
✓ 已验证
DOI
高影响因子
ORGANOMETALLICS
·
2020
·
IF 3.804
Liangwei Zhang,Long Liu,Tianzeng Huang,Qizhi Dong,Tieqiao Chen
A palladium-catalyzed cyclobutanation of aryl sulfonates with strained alkenes has been developed. The methodology is featured to achieve the cleavage of both C–O and C–H bonds of phenol derivatives in one pot. Under the reaction conditions, in addition to reactive triflates, the relatively inactive tosylates and mesylates can also be transformed into the corresponding benzocyclobutanes in high yields. This reaction can be carried out in gram-scale experiments with a low loading of the palladium catalyst and is applicable to the cyclobutanative modification of bioactive molecules, highlighting its synthetic value in organic synthesis.
研究领域:
有机化学
·
催化化学
·
合成化学
✓ 已验证
DOI
高影响因子
危险品化学品经营许可证（带存储）