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Improved reversed phase liquid chromatographic method with pulsed electrochemical detection for tobramycin in bulk and pharmaceutical formulation

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Journal of Pharmaceutical Analysis 2013年第3期3卷 161-167页

作者： Vicky Manyanga Ehab Elkady jos hoogmartens Erwin Adams Laboratory for Pharmaceutical Analysis Faculteit Farmaceutische Wetenschappen KU LeuvenO&N2 PB 923 Herestraat 49 B-3000 Leuven Belgium Pharmaceutical Chemistry Department Faculty of Pharmacy Cairo University Kasr El-Aini St.Cairo 11562 Egypt

Tobramycin is one of the aminoglycoside antibiotics that lack a UV absorbing chromophore. However, the application of pulsed electrochemical detection （PED） has been used successfully for the analysis of this and similar antibiotics. This work describes an improved liquid chromatographic （LC） method combined with PED, which is able to separate much more impurities than before. Using a Discovery C-18 RP column （250 mm × 4.6 mm i.d., 5 μm）, isocratic elution was carried out with a mobile phase, containing sodium sulfate （35 g/L）, sodium octanesulphonic acid （1 g/L）, tetrahydrofuran （14mL/L） and 0.2 M phosphate buffer pH 3.0 （50 mL/L）. Using these experimental conditions, the limit of quantification （LOQ, S/N= 10） was 5 ng. The linearity was examined in the range LOQ-60 μg/mL and the coefficient of determination was 0.998. The method also proved to be repeatable and the recovery was close to 100%. The influence of the different chromatographic parameters on the separation was investigated by means of an experimental design. The proposed method is useful in quality control of tobramycin drug substances and drug products.

关键词： Liquidchromatography-Pulsed electrochemicaldetection Tobramycin Aminoglycosideantibiotics

色谱柱分类数据库用于指导天然药物化学对照品色谱纯度测定时色谱柱理性选择（英文）

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色谱 2017年第2期35卷 196-202页

作者：王明娟戴忠马双成金红宇 hoogmartens jos ADAMS Erwin 中国食品药品检定研究院中药民族药检定所北京100050 鲁汶大学药物分析实验室

由于中药化学对照品多数来源于动植物药材,很容易混有结构类似物,故有机杂质测定是可能影响其化学对照品赋值准确性的关键风险因素。中药化学对照品的有机杂质测定通常采用药典收载或文献报道的高效液相色谱法,这些方法通常仅规定"以十... 详细信息

由于中药化学对照品多数来源于动植物药材,很容易混有结构类似物,故有机杂质测定是可能影响其化学对照品赋值准确性的关键风险因素。中药化学对照品的有机杂质测定通常采用药典收载或文献报道的高效液相色谱法,这些方法通常仅规定"以十八烷基硅烷键合硅胶为填充剂",无适宜色谱柱的品牌信息,或者实验室无文献所用的色谱柱品牌,而目前市场上已有800多种品牌的C18柱,生产工艺的不同导致不同品牌C18柱的选择性有差异,甚至差异显著。这很容易出现由于色谱柱选择不适宜而导致测定结果不准确的风险。该文采用国外色谱柱分类数据库指导对照品纯度考察时色谱柱的理性选择,尽可能减少色谱柱盲选可能导致的纯度结果不准确的风险。首先,用数据库挑选2根选择性差异显著的色谱柱(选择性因子F≥6)进行平行实验,以尽可能反映采用不同品牌色谱柱可能出现的分离效果差异。如果这2根色谱柱的分离效果及纯度测定结果无显著性差异,则可以交叉验证该对照品纯度测定的准确性。否则需要从数据库中选择另外1根与之前试验中分离效果更好、选择性相似的色谱柱进行纯度结果验证。在N-反式-p-对香豆酰基酪胺和表儿茶素没食子酸酯首批对照品的纯度考察中,使用了上述策略并验证了其有效性和科学性,计划推广应用至更多的中药化学对照品,特别当其可能含碱性或弱酸性化合物时,更应该尝试采用本文推荐的色谱柱选择策略交叉验证其纯度测定结果的准确性。

关键词：中药化学对照品色谱纯度色谱柱理性选择策略色谱柱分类数据库 N-反式-P-对香豆酰基酪胺表儿茶素没食子酸酯

Facilitated column selection in the separation of acetylspiramycin components using a simple column classification system

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Journal of Chinese Pharmaceutical Sciences 2011年第6期20卷 572-577页

作者：王明娟郑超胡昌勤金少鸿 hoogmartens jos VanSchepdael Ann Adams Erwin 中国食品药品检定研究院北京100050 鲁汶大学药物分析实验室重庆大学生物工程学院四川重庆400030

Acetylspiramycin（ASPM）,a 16-membered basic macrolide antibiotic,is the acetylated derivative of *** addition to the four main components,more than seventy minor components could be present in ***,it is a challenge to obtain a baseline separation of ASPM ***,in some cases it was found that the results obtained by different brands of C_（18） columns were significantly different,indicating the necessity of a rational column selection for the separation of ASPM *** this paper,we attempted to facilitate column selection for the analysis of ASPM using the database of the column characterization system established by Leuven *** the CAPCELL PAK MG C_（18）（250 mm×4.6 mm,5μm） as the reference column,three groups of columns（F2 group：similar selectivity;2F6：intermediate ranked group;F6 group： different selectivity,compared to the reference column） were selected,and their performances in the separation of ASPM components were evaluated under the chromatographic conditions described in Chinese Pharmacopoeia monograph.A good relationship was demonstrated between the ranking of columns and their selectivity in the separation of ASPM components,indicating the column classification system established by Leuven University was a helpful tool in the selection of suitable columns for the analysis of ASPM,a complex mixture of basic compounds.

关键词： Acetylspiramycin Semi-synthetic antibiotic Column selection Column characterization system

甲硝唑光降解杂质的研究及对药典有关物质方法的优化建议

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药物分析杂志 2022年第9期42卷 1667-1674页

作者：陈美玲许红霞袁伟峰赵隋红李雪朱兰新谌宗永刘宇晶马昂王明娟 hoogmartens jos ADAMS Erwin 北京阳光诺和药物研究股份有限公司北京102200 鲁汶大学药物分析实验室鲁汶B3000

目的:对采用现有各国药典中甲硝唑有关物质方法考察甲硝唑强光照射影响因素试验出现的物料不平衡(甲硝唑降解程度明显高于有关物质增长幅度)的原因进行调查。方法:用液相色谱-二极管阵列检测-串联质谱法(LC PDA-MS)对强光破坏的甲硝唑... 详细信息

目的:对采用现有各国药典中甲硝唑有关物质方法考察甲硝唑强光照射影响因素试验出现的物料不平衡(甲硝唑降解程度明显高于有关物质增长幅度)的原因进行调查。方法:用液相色谱-二极管阵列检测-串联质谱法(LC PDA-MS)对强光破坏的甲硝唑水溶液及其复方阴道洗剂的光降解产物进行定性鉴别和紫外光谱研究;用推导结构(N-(2-羟乙基)-5-甲基-l, 2,4-(口恶)二唑-3-甲酰胺)的杂质对照品,通过与甲硝唑光降解杂质保留时间和提取PDA光谱的一致性对比,及与甲硝唑氢谱的平行比较,对推导的甲硝唑光降解杂质结构进行确证;根据定性和光谱研究结果,依据现有药典方法优化了能同时检测该光降解杂质的方法并进行全面方法学验证。结果:甲硝唑在溶液、紫外光照条件下容易发生光降解,该杂质最大吸收约在230 nm,而在各论项下有关物质方法中设置的315/319 nm处吸收强度很弱。已上市甲硝唑注射液(需要缓慢输液)在室温光照条件下放置48 h或在5 000 lx条件下处理2 d和5 d后,光降解产物的量从“未检出”快速增加至0.15%、0.36%和0.88%,均超过本品的鉴定限(0.10%)和界定限(0.15%)。用230 nm检测并引入梯度洗脱、在各论项方法基础上优化建立的方法,能同时检测该光降解杂质和甲硝唑特定杂质2-甲基-5-硝基咪唑,方法的专属性、灵敏度、精密度、溶液的稳定性等指标均满足要求。结论:通过对甲硝唑光降解杂质的结构鉴定和光谱特征研究,揭示了采用现有药典检查方法考察甲硝唑光破坏样品出现的物料不平衡原因;建立了能同时控制该光降解杂质和甲硝唑现有特定杂质的优化方法;甲硝唑注射液慢速输液过程存在较大的光降解风险,需引起关注。

关键词：甲硝唑光降解风险评估结构鉴定串联质谱氢谱定量检测方法优化

Presynaptic endoplasmic reticulum architecture and hereditary spastic paraplegia

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Neural Regeneration Research 2024年第3期19卷 485-486页

作者： Juan joséPérez-Moreno Instituto de Biomedicina de Sevilla(IBiS) Hospital Universitario Virgen Del Rocío/CSIC/Universidad de Sevillaand Departamento de Biología CelularFacultad de BiologíaUniversidad de SevillaSevilleSpain

Hereditary spastic paraplegia(HSP)is a clinically and genetically heterogeneous neurodegenerative disorder,characterized primarily by progressive spasticity and weakness in the lower *** ients can also experience peripheral neuropathy,cognitive impairment,and other neurological *** date,more than 80 genes have been implicated in HSP,encompassing various cellular components,although mutations in genes encoding endoplasmic reticulum(ER)-shaping proteins are the most prevalent(Parodi et al.,2017).ER-shaping proteins are generally known for regulating the tubulation and curvation of the ER,but most of them show additional functions,including fusion of ER tubules,microtubule-severing,ER autophagy,lipid droplet synthesis,contact sites with other organelles(Öztürk et al.,2020).This highlights the complexity of studying the role of these proteins and the link between ER function and HSP.

关键词： reticulum endoplasmic

Fast synthesis of gold nanoparticles by cold atmospheric pressure plasma jet in the presence of Au^(+) ions and a capping agent

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Plasma Science and Technology 2024年第7期26卷 108-115页

作者： Tatiana HABIB josé Mauricio A.CAIUT Bruno CAILLIER Laboratoire Diagnostics des Plasmas Hors Equilibre(DPHE) Universitéde ToulouseINU ChampollionAlbi 81000France Department of Chemistry The Nanomaterials and Luminescent Systems GroupFaculty of PhilosophyScience and Letters at Ribeirão PretoUniversity of São PauloRibeirão Preto-SP 14040-901Brazil

Homogeneous gold nanoparticles were synthesized under atmospheric pressure using a nonthermal helium plasma jet in a single-step process.A current power supply was used to generate the plasma discharge rich in diverse reactive *** species induce rapid chemical reactions responsible for the reduction of the gold salts upon contact with the liquid *** this study,spherical and monodispersed gold nanoparticles were obtained within 5 min of plasma exposure using a solution containing gold(Ⅲ)chloride hydrate(HAuCl_(4))as a precursor and polyvinylpyrrolidone(PVP)as a capping agent to inhibit *** formation of these metal nanoparticles was initially perceptible through a visible change in the sample's color,transitioning from light yellow to a red/pink *** was subsequently corroborated by UVvis spectroscopy,which revealed an optical absorption in the 520-550 nm range for Au NPs,corresponding to the surface plasmon resonance(SPR)*** investigation into the impact of various parameters,including plasma discharge duration,precursor and capping agent concentrations,was carried out to optimize conditions for the formation of well-separated,spherical gold *** light scattering(DLS)was used to measure the size of these nanoparticles,transmission electron microscopy(TEM)was used to observe their morphology and X-ray diffraction(XRD)was also employed to determine their crystallographic *** results confirm that homogeneous spherical gold nanoparticles with an average diameter of 13 nm can be easily synthesized through a rapid,straightforward,and environmentally friendly approach utilizing a helium atmospheric pressure plasma.

关键词： gold nanoparticles non-thermal plasma jet helium DBD

Capsule endoscopy and panendoscopy:A journey to the future of gastrointestinal endoscopy

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World Journal of Gastroenterology 2024年第10期30卷 1270-1279页

作者： Bruno Rosa joséCotter Department of Gastroenterology Hospital da Senhora da OliveiraGuimarães 4835-044Portugal Life and Health Sciences Research Institute School of MedicineUniversity of MinhoBraga 4710-057Portugal ICVS/3B's PT Government Associate LaboratoryBraga 4710-057Portugal

In 2000,the small bowel capsule revolutionized the management of patients with small bowel ***,the technological development achieved by the new models of double-headed endoscopic capsules,as miniaturized devices to evaluate the small bowel and colon[pan-intestinal capsule endoscopy(PCE)],makes this non-invasive procedure a disruptive concept for the management of patients with digestive *** technology is expected to identify which patients will require conventional invasive endoscopic procedures(colonoscopy or balloon-assisted enteroscopy),based on the lesions detected by the capsule,i.e.,those with an indication for biopsies or endoscopic *** use of PCE in patients with inflammatory bowel diseases,namely Crohn’s disease,as well as in patients with iron deficiency anaemia and/or overt gastrointestinal(GI)bleeding,after a non-diagnostic upper endoscopy(esophagogastroduodenoscopy),enables an effective,safe and comfortable way to identify patients with relevant lesions,who should undergo subsequent invasive endoscopic *** recent development of magnetically controlled capsule endoscopy to evaluate the upper GI tract,is a further step towards the possibility of an entirely non-invasive assessment of all the segments of the digestive tract,from mouth-to-anus,meeting the expectations of the early developers of capsule endoscopy.

关键词： Non-invasive endoscopy Panendoscopy Magnetically controlled capsule endoscopy Crohn’s disease Digestive bleeding

Taurine as a possible therapy for immunosenescence and inflammaging

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Cellular & Molecular Immunology 2024年第1期21卷 3-5页

作者： joséM.Izquierdo Centro de Biología Molecular Severo Ochoa(CBMSO).Consejo Superior de Investigaciones Científicas Universidad Autónoma de Madrid(CSIC/UAM)C/Nicolás Cabrera 1Campus de Cantoblanco28049MadridSpain

In their recent Science article,Singh et *** taurine as an endogenously produced anti-inflammatory,anti-immunosenescence,and anti-aging *** authors also show that restoring taurine to its“youthful”levels prevents in... 详细信息

关键词： Taurine inflam

Tracking the change in Spanish greenhouse gas emissions through an LMDI decomposition model:A global and sectoral approach

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Journal of Environmental Sciences 2024年第5期139卷 114-122页

作者： Paula Fernández González María josé Presno Manuel Landajo Department of Applied Economics University of OviedoAuda del Cristos/n 33011 OviedoSpain

The reduction of GHG emissions to reverse the greenhouse effect is one of the main challenges in this *** this paper we pursue two ***,we analyze the evolution of GHG emissions in Spain in 2008–2018,at both the global and sectoral levels,with the variation in emissions decomposed into a set of determining ***,we propose several actions specifically oriented to more tightly controlling the level of *** results showed a remarkable reduction(18.44%)in GHG emissions,mainly due to the intensity effect,but also to the production-per-capita *** detected somewhat different patterns among the various sectors *** the intensity effect was the most influential one in the agricultural,transport,and others sectors,the production-per-capita effect was predominant in the case of *** carbonization effect was revealed as crucial in the commerce *** above findings highlight the importance of the energy efficiency measures taken in recent years in the Spanish economy,also pointing to the need to deepen those strategies and to propose new measures that entail greater efficiency in *** efforts in areas like innovation,R&D,diffusion of more eco-friendly technologies,and a greater use of greener energies all prove to be essential reduction actions to fight the greenhouse effect.

关键词： LMDI Decomposition Spain GHG emissions