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Rapid discovery and identification of 68 compounds in the active fraction from Xiao-Xu-Ming decoction(XXMD) by HPLC-HRMS and MTSF technique

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Chinese Chemical Letters 2014年第12期25卷 1648-1652页

作者： Cai-Hong Wang Cai-Sheng Wu Hai-Lin Qin Jin-Lan Zhang State Key Laboratory of Bioactive substance and Function of Natural Medicines.Institute of Materia Medica Chinese Academy of Medical Sciences  Peking Union Medical College State Key Laboratory of Bioactive substance and Function of Natural Medicines.Institute of Materia Medica Chinese Academy of Medical Sciences Peking Union Medical College

Xiao-Xu-Ming decoction（XXMD） was a traditional Chinese prescription and first recorded in ＂Bei Ji Qian Jin Yao Fang＂.It has been widely used to treat theoplegia and the sequel of theoplegia in *** the present work,high-performance liquid chromatography coupled with high resolution mass spectrometry（HPLC-HRMS） combined with the mass spectral tree similarity filter technique（MTSF）was used to rapidly discover and identify the compounds of the active fraction of XXMD.A total of 3362 compounds were automatically detected by HPLC-HRMS,and final 68 compounds were identified in the active fraction of *** 14 templated compounds（reference compounds）,50 related compounds fished by MTSF technique,and 4 unrelated compounds identified by manual *** study successfully applied MTSF technology for the first time to discover and identify the components of Chinese *** results demonstrated that MTSF technique should be useful to the discovery and identification of compounds in Chinese *** study also proved that MTSF can be applied to the targeted phytochemical separation.

关键词： Xiao-Xu-Ming decoction High-performance liquid chromatography with high resolution mass spectrometry Mass spectral trees similarity filter technique

Separation and identification of moxifloxacin impurities in drug substance by high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform ion cyclotron resonance mass spectrometry

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Chinese Chemical Letters 2012年第10期23卷 1185-1188页

作者： Cai Sheng Wu Zhi Xin Jia Bao Ming Ning Jin Lan Zhang Song Wu State Key Laboratory of Bioactive substance and Function of Natural Medicines Institute of Materia Medica Chinese Academy of Medical Sciences & Peking Union Medical College Beijing 100050 China Institute of Materia Medica Chinese Academy of Medical Sciences & Peking Union Medical College Beijing 100050 China National Institutes for Food and Drug Control Beijing 100050 China

In this paper, a high-performance liquid chromatography coupled with ultraviolet detection and Fourier transform-ion cyclotron resonance mass spectrometry （HPLC-UV/FrICRMS） method was described for the investigation of impurity profile in moxifloxacin （MOX） drug substance and chemical reference substance. Ten impurities were detected by HPLC-UV, while eight impurities were identified by using the high accurate molecular mass combined with multiple-stage mass spectrometric data and fragmentation rules. In addition, to our knowledge, five impurities were founded for the first time in MOX drug substance.

关键词： Moxifloxacin (MOX) Impurity profile High-performance liquid chromatography coupled with ultraviolet detection and Fouriertransform-ion cyclotron resonance mass spectrometry (HPLC-UV/bTICRMS)

Single-run reversed-phase HPLC method for determining sertraline content,enantiomeric purity,and related substances in drug substance and finished product

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Journal of Pharmaceutical Analysis 2020年第6期10卷 610-616页

作者： Alessia Rosetti Rosella Ferretti Leo Zanitti Adriano Casulli Claudio Villani Roberto Cirilli National Centre for the Control and Evaluation of Medicines Chemical Medicines UnitIstituto Superiore di Sanita(ISS)Viale Regina Elena 29900161RomeItaly Department of Chemistry and Technology of Drugs Sapienza University of Rome00185RomeItaly WHO Collaborating Centre for the Epidemiology Detection and Control of Cystic and Alveolar EchinococcosisEuropean Union Reference Laboratory for ParasitesIstituto Superiore di Sanita(ISS)Viale Regina Elena 29900161RomeItaly

A direct enantio-,diastereo-,and chemo-selective high-performance liquid chromatographic method was developed for determining the content,enantiomeric purity,and related substances of the chiral antidepressant drug sertraline HCl in a single chromatographic *** separation was achieved on a chiral stationary phase based on amylose tris(3-chloro-5-methylphenylcarbamate)under reversed-phase *** method was optimized by evaluating the influence of the temperature and mobile phase composition on the retention and *** application of the single-run approach allowed to baseline resolve all investigated species in less than 15 min,without using buffers or tandem-coupled *** chromatographic method was validated according to the guidelines of the Official Medicines Control Laboratory and applied to control the content of sertraline HCl and related chiral substances in a generic antidepressant formulation.

关键词： Chiralpak IG-3 Enantiomers Diastereomers Reversed-phase enantioselective HPLC Sertraline HCl

Isolation and identification of human metabolites from a novel anti-tumor candidate drug 5-chlorogenic acid injection by HPLC-HRMS/MSn and HPLC-SPE-NMR

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Isolation and identification of human metabolites from a nov...

The pharmacokinetic and tissue distribution study of Chuanhuning liposomes in rats

第三届全国质谱分析学术报告会

作者： Tiankun Ren Yanan Wang Caihong Wang Mengtian Zhang Wang Huang Jiandong Jiang Wenbin Li Jinlan Zhang State Key Laboratory of Bioactive substance and Function of Natural Medicines Institute of Materia Medica Peking Union Medical College & Chinese Academy of Medical Sciences Jiuzhang Biochemical Engineering Science and Technology Development Co. Ltd. Department of Glioma Beijing Shijitan Hospital Capital Medical University

A novel anti-tumor candidate drug, 5-Chlorogenic acid（5-CQA） injection, was used for the treatment of malignant glioma in clinical trial（phase I） in China. The isolation and identification of the metabolites of 5-CQA injection in humans were investigated in the present study. Urine and feces samples obtained after intramuscular administration of 5-CQA injection to healthy adults have been analyzed by high-performance liquid chromatography coupled with high resolution mass and multiple-stage mass spectrometer（HPLC-HRMS/MSn）. No metabolite was detected in human feces, however in human urine, a total of 6 metabolites were identified including isomerized 5-CQA（P1 and P2）, hydrolyzed 5-CQA（M1 and M2）, as well as methylated 5-CQA（M3 and M4）. Among them, M3 and M4 were main metabolites and target analytes for human mass balance study. Additional, the structure of M3 and M4 was characterized by high performance liquid chromatography-solid phase extraction-nuclear magnetic resonance（HPLC-SPE-NMR）, and the results demonstrated that the methoxy group of M3 and M4 was exclusively attributed to C-3’ and C-4’, respectively. Due to the unavailable of commercial reference, the pure products of M3 and M4 were synthesized by 5-CQA methylation and followed by isolation and purification. Moreover, the potential activity of M3 and M4 on malignant glioma was predicted using a reverse molecular docking analysis on eight malignant glioma-related pathways. The results showed that M3 and M4 had a various interactions against malignant glioma-related targets. Our study provides the insight into the metabolism of 5-CQA injection in humans and supports the clinical human mass balance study（Fig. 1）.

关键词： 5-Chlorogenic acid(5-CQA) Identification HPLC-HRMS/MSn HPLC-SPE-NMR

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The pharmacokinetic and tissue distribution study of Chuanhu...

Assessment of Acute Poisoning Cases in Emergency Department of the Provincial General reference Hospital in Bukavu, DR-Congo

“好医生杯”中药制剂创新与发展论坛

作者：禹玉洪 Qiao Foxiao Xuan Jingji Li Yunqing Li Yan 亚宝药业集团股份有限公司 Yabao Pharmaceutical Group limited Beijing pharmaceutical research Institute State Key Laboratory of Bioactive substance and Function of Natural Medicines Institute of Materia MedicaChinese Academy of Medical Sciences and Peking Union Medical College

Liposome has the ability of reducing side effects and drug dosage,and a growing number of liposomes are used in drug research and *** injection has obvious anti-inflammatory,antipyretic,promote adrenocortical function and sedation,which is widely used in treatment of viral pneumonia and viral upper respiratory tract ***,more and more reports were published about its clinical adverse *** purpose of this study is to research the pharmacokinetics and tissue distribution of Chuanhuning-liposome injection(CHL)in ***:High pressure homogenization method was used to prepare *** commercial ordinary Chuanhuning injection was used as the reference to evaluate the pharmacokinetics and tissue distribution of *** pharmacokinetic and tissue distribution was studied in rats after intravenous administration at 40 mg/kg and the concentration of dehydroandrographolide succiuate(DAS,the active ingredients of CHL in vivo)was detected by LC-MS/*** analysis was performed using non-compartmental model via proprietary DAS 2.0(Drug and Statistics)computer software *** relative tissue exposure values(RE)were used to evaluate the tissue targeting of ***:We prepared three batches of qualified good stability CHL consecutively,which size was smaller than 100 nm and its encapsulation rate was as high as 98.2%.First,a suitable detection method was set up to study the pharmacokinetic of *** MS recordings were carried out in multiple reaction monitoring(MRM)*** were monitored at m/z 531.2→99 for DAS and m/z267.1→252 for formononetin(IS).The calibration curves ranged from 5 to 4000 ng/ml,and the LLOQ was 5 ng/***-day and inter-day precision were less than 4.26%.The intra-day and inter-day accuracy were within±9.3%,and the recovery ranged from 83.79%to 94.77%.The average of AUC(0-t),MRT(0-oo)and CLz were 29488.82μg/L*h,0.58 h and 1.61 L/h/kg for CHL and 43540.93μg/L*h,1.87 h and 1.05 L/h/k

关键词： pharmaceutics dehydroandrographolide succinate liposome pharmacokinetics tissue distribution

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Advances in Infectious Diseases 2023年第2期13卷 233-248页

作者： Billy Paul Kaishusha Mupendwa Espoir Batumike Murhi Guy Mulumeoderhwa Mulinganya Mannix Masimango Imani Kesner Mateso Salama Kaishusha David Justin-Leonard Kadima Ntokamunda Elie Batulani Mushosi-Tamba Faculty of Natural Health Science Bircham International University Department of Toxicology Madrid Spain The Provincial General reference Hospital of Bukavu Bukavu Democratic Republic of the Congo Department of Pharmacy Official University of Bukavu (U.O.B) Bukavu Democratic Republic of the Congo Department of Anesthesiology at Félix Houphouë t Boigny University (UFHB) Abidjan Ivory Coast

Background: Acute intoxications result from intentionally or accidentally taking a relatively significant amount of a chemical substance which triggers disturbances in the level of psychophysiological functions, the complications of which may lead to mental disorders, physical causalities, and death. Any acute intoxication mostly requires emergency care. Objective: To highlight the prevalence, history, clinical features, emergency treatment, and prediction of acute intoxication cases referred to the emergency services at the Provincial General reference Hospital in Bukavu, DR-Congo. Methods: A retrospective cross-sectional study was conducted from January 2021 to October 2022 based on an analysis of patients’ medical files. Triage was performed among all-type of patient files recorded in the computerized hospital database Ebale-Sante to sort cases of intoxication. Results: During the observational period, 3966 emergency admissions were counted, of which 321 (8.09%) patients were identified as having acute intoxication. Among these, 100 files that containing sufficient information fit the quality criteria for this study’s analysis. The victims were infants, adolescents and adults aged 1 - 45 years, and 52% were female and 48% were male. Most cases were accidental and, occurred at home, and the victims were driven to the hospital within 2 - 24 hours. The substances consumed included household products, drugs, and herbs. Resuscitation care, antidotes and supportive symptomatic medications ensured that 85% were healed and 10% experienced sequelae;however, 5% died. Conclusion: Acute intoxication occurs in infants mostly accidentally though the ingestion of household products and medicines. Furthermore, suicide cases may occur in traumatized adolescents and discordant couples. People should be informed about how to store hazardous products (e.g.: drugs, household products and pesticides), which should not be available to children, to avoid unintentional poisoning. Special

关键词： Acute Intoxication Patients Emergency Provincial General reference Hospital Bukavu

A new procedure combining GC-MS with accelerated solvent extraction for the analysis of phthalic acid esters in contaminated soils

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Frontiers of Environmental Science & Engineering 2013年第1期7卷 31-42页

作者： Tingting MA Ying TENG Peter CHRISTIE Yongming LUO Yongshan CHEN Mao YE Key Laboratory of Soil Environment and Pollution Remediation Institute of Soil Science Chinese Academy of Sciences Nanjing 210008 China Graduate University of the Chinese Academy of Sciences Beijing 100049China Agri-Environment branch Agri-Food and Biosciences Institute Newforge Lane Belfast BT9 5PX United Kingdom State key Laboratory of Environment Simulation and Pollution control (Jomt) Tsinghua University Beijing 100084 China State Key Laboratory of Soil and Sustainable Agriculture Institute of Soil Science Chinese Academy of Sciences Nanjing 210008 China

An optimized procedure based on gas chromatography-mass spectrometry (GC-MS) combined with accelerated solvent extraction (ASE) is developed for the analysis of six phthalic acid esters (PAEs), which are priority soil pollutants nominated by United States Environmental Protection Agency (USEPA). Quantification of PAEs in soil employs ultrasonic extraction (UE) (USEPA 3550) and ASE (USEPA 3545), followed by clean up procedures involving three different chromatography columns and two combined elution methods. GC-MS conditions under selected ion monitoring (SIM) mode are described and quality assurance and quality control (QA/QC) criteria with high accuracy and sensitivity for target analytes were achieved. Method reliability is assured with the use of an isotopically labeled PAE, di- -butyl phthalate-d4 (DnBP-D4), as a surrogate, and benzyl benzoate (BB) as an internal standard, and with the analysis of certified reference materials (CRM). QA/QC for the developed procedure was tested in four PAE-spiked soils and one PAE-contaminated soil. The four spiked soils were originated from typical Chinese agricultural fields and the contaminated soil was obtained from an electronic waste dismantling area. Instrument detection limits (IDLs) for the six PAEs ranged 0.10–0.31 μg·L and method detection limits (MDLs) of the four spiked soils varied from a range of 20–70 μg·kg to a range of 90– 290 μg·kg . Linearity of response between 20 μg·L and 2 mg·L was also established and the correlation coefficients ( ) were all>0.998. Spiked soil matrix showed relative recovery rates between 75 and 120% for the six target compounds and about 93% for the surrogate substance. The developed procedure is anticipated to be highly applicable for field surveys of soil PAE pollution in China.

关键词： phthalic acid esters quality assurance and quality control soil type accelerated solvent extraction certified reference materials