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Measurement of Arsenic Species in Infant Rice Cereals by Liquid Chromatography Inductively Coupled Plasma Mass Spectrometry 被引量:2
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作者 John D. Brockman John W. N. Brown IV 《American Journal of Analytical Chemistry》 2012年第10期693-697,共5页
Infant rice cereals were analyzed for total arsenic, inorganic arsenic (i-As) and the organic arsenic species monomethylarsonoic acid (MMA) and dimethylarsinic acid (DMA) using liquid chromatography inductively couple... Infant rice cereals were analyzed for total arsenic, inorganic arsenic (i-As) and the organic arsenic species monomethylarsonoic acid (MMA) and dimethylarsinic acid (DMA) using liquid chromatography inductively coupled plasma mass spectrometry (LC-ICP-MS). Total arsenic concentrations in the samples ranged from 110 ng/gup to 420 ng/g. The i-As in the rice cereals accounted for 33% to 77% of the total arsenic. The observed variability between infant rice cereals makes a dietary survey approach to accessing arsenic exposures difficult. 展开更多
关键词 Arsenic SPECIATION Epidemiology INFANT RICE CEREAL liquid chromatography Inductively coupled Plas-ma mass Spectrometry
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Rapid Screening of 26 Organophosphorus Pesticides in Fresh Milk by Ultra Liquid Chromatography Coupled With Quadrupole-Time of Flight Mass Spectrometry 被引量:1
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作者 Yi LI Luman HUO +4 位作者 Lei WANG Lixue DONG Aijun LI Yi ZHANG Baiqin ZHENG 《Agricultural Biotechnology》 CAS 2021年第5期131-133,共3页
[Objectives]A rapid screening and analysis method for 26 organophosphorus agrochemicals in fresh milk was established using ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrome... [Objectives]A rapid screening and analysis method for 26 organophosphorus agrochemicals in fresh milk was established using ultra performance liquid chromatography coupled with quadrupole-time of flight mass spectrometry.[Methods]Raw milk was extracted with acetonitrile solution containing 0.2%formic acid by volume,and purified with a Dikma ProElut QuECHERS solid phase extraction cartridge.Target compounds were separated on a Waters ACQUITY UPLC HSS T3 chromatographic column(2.1 mm×50 mm,1.8μm)with methanol-water solution as a mobile phase for gradient elution,and through scanning with an electrospray ion source in positive ion mode,26 kinds of organophosphorus agrochemicals could be accurately qualitatively determined within 10 min.[Results]When using formic acid acetonitrile with a volume fraction of 0.2%,there were more types of detected compounds and a greater recovery;and using B cartridge could effectively eliminate the interference of non-polar substances such as phospholipids,achieve higher number of detected compounds than those of A and C,and well separate the 26 kinds of agrochemical residues.[Conclusions]This study provides a reference method for the rapid screening of agrochemical residues in dairy cows in the future. 展开更多
关键词 Ultra liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF-MS) Fresh milk Organophosphorus agrochemicals Rapid screening
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Lysophosphatidylcholine Biomarkers of Lung Cancer Detected by Ultra-performance Liquid Chromatography Coupled with Quadrupole Time-of-flight Mass Spectrometry
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作者 DONG Jun CAI Xiao-ming +4 位作者 ZOU Li-juan CHEN Cheng XUE Xing-ya ZHANG Xiu-li LIANG Xin-miao 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2011年第5期750-755,共6页
Centrifugal ultrafiltration after methanol extraction of whole plasma was used as an optimal condition for the preparation of blood plasma before metabonomic studies. The plasma samples from 102 lung cancer patients a... Centrifugal ultrafiltration after methanol extraction of whole plasma was used as an optimal condition for the preparation of blood plasma before metabonomic studies. The plasma samples from 102 lung cancer patients and 34 healthy volunteers were prepared with this approach. With ultra-performance liquid chromatography(UPLC) coupled with quadrupole time-of-flight mass spectrometry(Q-TOF MS) analysis, the samples were investigated in order to find potential disease biomarkers. After data acquisition, orthogonal signal correction partial least squares models were built to differentiate the healthy volunteers from lung cancer patients and to identify metabolites that showed significantly different expression between the two groups. Several metabolite ions were identified as potential biomarkers according to the variable importance in the project(VIP) value in both ion modes. Five lysophosphatidylcholines were further identified as specifically lysoPC 16:0, isomer of lysoPC 16:0, lysoPC 18:0, lysoPC 18:1 and lysoPC 18:2. These results suggest that UPLC coupled with Q-TOF MS is an effective technique for the analysis of plasma metabolites in metabonomic studies. 展开更多
关键词 METABONOMICS Sample preparation Ultra-performance liquid chromatography coupled with quadrupoletime-of-flight mass spectrometry(UPLC/Q-TOF MS) Lung cancer Biomarker
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Effect of pediatric tuina on hypothalamic metabolites in young rabbits using liquid chromatography-mass spectrometry 被引量:1
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作者 Zhifeng Liu Yi Jiao +7 位作者 Tianyuan Yu Yingqi Zhang Di Liu Hourong Wang Yajing Xu Qian Guan Taotao Lv Jian Shu 《Journal of Traditional Chinese Medical Sciences》 2022年第2期188-196,共9页
Objective: To investigate the changes in the hypothalamic metabolites of lipopolysaccharide(LPS) febrile young rabbits after the treatment with pediatric tuina.Methods: A total of 30 young rabbits were randomly assign... Objective: To investigate the changes in the hypothalamic metabolites of lipopolysaccharide(LPS) febrile young rabbits after the treatment with pediatric tuina.Methods: A total of 30 young rabbits were randomly assigned into three groups: the normal group, the model group, and the tuina group. Both the model group and the tuina group were injected intravenously with LPS. “Six antipyretic manipulations”(pushing Tianmen, pushing Kangong, kneading Taiyang,kneading Erhougaogu, clearing Tianheshui, and pushing Jizhu) were administered 1 h after the LPS injection in the tuina group. The rectal temperatures of the young rabbits were monitored during the experiment to explore the antipyretic effect. Three hours after the injection, the content of interleukin-1β(IL-1β), tumor necrosis factor(TNF)-a, and prostaglandin E;(PGE;) in the serum was detected. In addition, liquid chromatography-mass spectrometry(LC-MS) was used for the hypothalamus metabolomics.Results: Compared with the model group, the rectal temperature of the tuina group was decreased at 2 h and 3 h after the LPS injection(P =.04, P =.03, respectively), and the content of IL-1β, TNF-a, and PGE2was decreased(P =.03, P =.003, and P =.008, respectively). The metabolomics results showed that there were 23 potential biomarkers after the tuina intervention, enriching 27 pathways. Lipid metabolites,especially glycerophospholipids, were a majority of the altered metabolites. The primary metabolic pathways affected by tuina included the arachidonic acid metabolism, the GABAergic synapse, D-glutamine and D-glutamate metabolism, and the glutamatergic synapse.Conclusion: Pediatric tuina reduced the temperature of the febrile rabbits and downregulated the expression of IL-1β, TNF-a, and PGE2, and the antipyretic mechanism may be related to changes in metabolites and metabolic pathways in the hypothalamus. 展开更多
关键词 FEVER Pediatric tuina Metabolomics liquid chromatography coupled with mass spectrometry HYPOTHALAMUS INTERLEUKIN-1B Tumor necrosis factor-a Prostaglandin E_(2)
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土壤中Sb(Ⅲ)和Sb(Ⅴ)的有效提取与测定
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作者 陈皓 刘硕勋 +1 位作者 陈玲 杨超 《同济大学学报(自然科学版)》 EI CAS CSCD 北大核心 2024年第8期1270-1277,共8页
锑的各种形态中三价锑和五价锑的毒性较高,在城市土壤锑组成中占比也较高。研究了萃取方式、萃取剂、萃取条件、色谱分离流动相条件等因素对土壤中价态锑提取和分析的影响,建立了完整的土壤价态锑萃取-分析方法。研究推荐以柠檬酸溶液... 锑的各种形态中三价锑和五价锑的毒性较高,在城市土壤锑组成中占比也较高。研究了萃取方式、萃取剂、萃取条件、色谱分离流动相条件等因素对土壤中价态锑提取和分析的影响,建立了完整的土壤价态锑萃取-分析方法。研究推荐以柠檬酸溶液为萃取剂,70℃恒温振荡萃取的方式提取价态锑,萃取液以乙二胺四乙酸二钾+邻苯二甲酸为流动相,经色谱分离后利用电感耦合等离子体质谱仪对不同价态的Sb进行分析。所建立的方法检出限低,准确性精密度好,可用于实际土壤样品中价态锑的有效提取与测定。 展开更多
关键词 价态锑 道路土壤 试剂萃取 液相色谱-电感耦合等离子体质谱联用法
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A rapid and simple ultraperformance liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS) method for the detection of glucuronic acid-conjugated steroid metabolites
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作者 戎怿 黄碧云 +2 位作者 黄珺珺 朱柳 刘夏雯 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2016年第4期291-301,共11页
In the present study, we effectively detected 10 steroids and glucuronic acid-conjugated steroid metabolites in 12 min by ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Ster... In the present study, we effectively detected 10 steroids and glucuronic acid-conjugated steroid metabolites in 12 min by ultraperformance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS). Steroids testosterone (T), 5ct-dihydrotestosterone (DHT), androsterone (ADT), etiocholanolone (ETIO), estradiol (E2) and their glucuronide conjugates were well-separated on an Eclipse Plus C18 column (2.1 mm×50 ram, RRHD 1.8μm). The mobile phase consisted of a mixture of methanol and ultrapure water (containing I mM ammonium formate) at a ratio of 60:40 (v/v), and the flow rate was set at 0.25 mL/min. The LC eluate was detected by electrospray ionization (ESI) source in both positive and negative ion modes. Neutral loss (NL of 176, 194, 211 and 229 Da in positive mode) and precursor ion (PI ofm/z 141,159 and 177 in positive mode and 75, 85 and 133 in negative mode) methods were applied for the detection of steroid glucuronides. The multiple reaction monitoring (MRM) transitions were m/z 289.3→97.1,291.3→105, 291.3→199.2, 273.2→145.4 and 255.2→159.1 for T, DHT, ADT, ETIO and E2 in positive mode, respectively; as well as m/z 463.3→85 for T glucuronide (T-G), m/z 465.3→75 for DHT glucuronide (DHT-G), ADT glucuronide (ADT-G), ETIO glucuronide (ETIO-G) and m/z 447.3→271 for E2 glucuronide (Ez-G) in negative mode. In addition, the analytical method was also applied for the detection of steroid glucuronides in pooled human liver microsomes (HLM), which might serve as a basis for further investigation of steroid metabolism in vivo and in vitro. 展开更多
关键词 Steroid glucuronides Ultraperformance liquid chromatography coupled to tandem mass spectrometry Human liver microsome
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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 被引量:8
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作者 Cai Sheng Wu Zhi Xin Jia +2 位作者 Bao Ming Ning Jin Lan Zhang Song Wu 《Chinese Chemical Letters》 SCIE CAS CSCD 2012年第10期1185-1188,共4页
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... 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. 展开更多
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)
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COMPREHENSIVE TWO-DIMENSIONAL LIQUID CHROMATOGRAPHY COUPLED WITH QUADRUPLE TIME-OF-FLIGHT MASS SPECTROMETRY FOR CHEMICAL CONSTITUENTS ANALYSIS OF TRIPTERYGIUM GLYCOSIDES TABLETS 被引量:11
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作者 Xiao Yao 《World Journal of Traditional Chinese Medicine》 2015年第4期66-66,共1页
Comprehensive two-dimensional liquid chromatography platform(LC×LC)coupled with quadrupole time-of-flight(QTOF)mass spectrometry(MS)is developed to separate,identify and relatively determine the chemical constitu... Comprehensive two-dimensional liquid chromatography platform(LC×LC)coupled with quadrupole time-of-flight(QTOF)mass spectrometry(MS)is developed to separate,identify and relatively determine the chemical constituents of two types of tripterygium glycosides tablets(TGT).The types and relative contents of the constituents discovered in two kinds of TGT tablets were subsequently compared.C8andC18 column were used for the separation of the first 展开更多
关键词 TGT COMPREHENSIVE TWO-DIMENSIONAL liquid chromatography coupled WITH QUADRUPLE TIME-OF-FLIGHT mass SPECTROMETRY FOR CHEMICAL CONSTITUENTS ANALYSIS OF TRIPTERYGIUM GLYCOSIDES TABLETS
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不同品种生菜的多酚、黄酮差异比较与抗氧化活性 被引量:2
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作者 余菲 赵晓燕 +3 位作者 周昌艳 魏仕伟 鄂恒超 李晓贝 《食品科学》 EI CAS CSCD 北大核心 2024年第13期17-25,共9页
生菜富含多种酚酸、黄酮类化合物,是获取膳食多酚的良好食物来源。本研究对50个不同品种(34种绿色品种和16种红色品种)生菜中的总酚、总黄酮含量及其抗氧化能力进行测定,同时采用超高效液相色谱-四极杆-飞行时间质谱法和超高效液相色谱... 生菜富含多种酚酸、黄酮类化合物,是获取膳食多酚的良好食物来源。本研究对50个不同品种(34种绿色品种和16种红色品种)生菜中的总酚、总黄酮含量及其抗氧化能力进行测定,同时采用超高效液相色谱-四极杆-飞行时间质谱法和超高效液相色谱法对生菜中17种特征酚酸和黄酮类化合物进行鉴定及含量测定,再结合多元统计分析进行分类和相关性分析。结果表明,红色品种生菜的总酚、总黄酮含量及抗氧化能力高于绿色品种生菜;50种生菜中鉴定出绿原酸、咖啡酸、异绿原酸A/B、菊苣酸、木犀草素-7-O-β-D-葡萄糖醛酸苷、槲皮素-3-O-葡萄糖酸苷和槲皮素-3-O-葡萄糖苷7种多酚类化合物,整体在红色品种生菜中含量更高。多元统计分析结果表明绿原酸、木犀草素-7-O-β-D-葡萄糖醛酸苷和槲皮素-3-O-葡萄糖苷与抗氧化能力的相关性较高。综上,G21K104、W3088、H20K6457等5个红色新品种及商业种,G21K212、G21K117等4个绿色新品种为高抗氧化活性生菜品种。本研究可为生菜育种、种质资源创新和营养健康、功能性产品开发提供参考依据。 展开更多
关键词 生菜 多酚 黄酮 抗氧化 超高效液相色谱法 超高效液相色谱-四极杆-飞行时间-质谱法 多元统计分析
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Pharmacokinetic Comparison of Four Major Bio-Active Components of Naoxintong Capsule in Normal and Acute Blood Stasis Rats Using Ultra-Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry 被引量:1
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作者 Wei-Xia Li Shu-Qi Zhang +5 位作者 Man-Man Li Hui Zhang Xiao-Yan Wang Lu Niu Jin-Fa Tang Xue-Lin Li 《World Journal of Traditional Chinese Medicine》 2022年第1期92-99,共8页
Objective: To compare the pharmacokinetic differences of the main components of Naoxintong capsule(NXTC) in normal and acute blood stasis rats. Materials and Methods: Rats were subcutaneously injected with adrenaline ... Objective: To compare the pharmacokinetic differences of the main components of Naoxintong capsule(NXTC) in normal and acute blood stasis rats. Materials and Methods: Rats were subcutaneously injected with adrenaline hydrochloride twice;during the two subcutaneous injections, the rats were placed in ice water for 4 min to reproduce the model rat of acute blood stasis. The normal and acute blood stasis rats were administrated a 5.04 g/kg dose of NXTC suspension. Then, blood samples were collected from the posterior retinal venous plexus at different time points. Plasma concentrations of four major bio-active components including caffeic acid, ferulic acid, formononetin, and tanshinone IIA in NXTC were measured using ultra-performance liquid chromatography coupled with triple-quadrupole mass spectrometry. Phoenix Win Nonlin v6.2 software was used to calculate the pharmacokinetic parameters. Results: Compared with the normal rats, the acute blood stasis rats showed a significant decrease in C_(max) of ferulic acid and formononetin, AUC_(all) of caffeic acid and ferulic acid, and AUC_(INF_obs) of ferulic acid. Conversely, an increase in the Vz_F_obs and MRT_(last) of ferulic acid and caffeic acid was observed. These findings demonstrate that the absorption of the four NXTC components was weakened in the acute blood stasis rats and that the elimination time was prolonged. Conclusions: The significant difference in some parameters of the four NXTC components between the normal and acute blood stasis rats might be caused by an increase in blood viscosity and the subsequent slowing down of blood flow in the acute blood stasis rats. The pharmacokinetic study conducted in pathological state can provide important information and scientific basis for further rational clinical application of NXTC. 展开更多
关键词 Acute blood stasis rat model Naoxintong capsules PHARMACOKINETICS ultra-performance liquid chromatography coupled with triple-quadrupole mass spectrometry
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Rapid Differentiation of Aconiti Kusnezoffii Radix from Different Geographic Origins Using Ultra-Performance Liquid Chromatography Coupled with Time-of-Flight Mass Spectrometry 被引量:1
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作者 En-Yu Lu Zi-Feng Pi +4 位作者 Zhong Zheng Shu Liu Feng-Rui Song Na Li Zhi-Qiang Liu 《World Journal of Traditional Chinese Medicine》 2021年第1期71-77,共7页
Objective:There are different geographic origins of Aconiti Kusnezoffii Radixs(AKRs)sold in the market with different quality.This study aims to establish a rapid analysis method to distinguish the different geographi... Objective:There are different geographic origins of Aconiti Kusnezoffii Radixs(AKRs)sold in the market with different quality.This study aims to establish a rapid analysis method to distinguish the different geographic origins of AKRs and to realize the rapid evaluation of their quality.Methods:An ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry(UPLC-Q-TOF MS)method was utilized to acquire the constituents'information of AKRs from different geographic origins.MSE data and Progenesis QI software were employed to identify the chemical constitutes.Principal component analysis(PCA)was applied to comparing MS data to find the chemical markers of AKRs from different geographic origins.Results:Twenty-three components were detected and 17 out of them were identified,including diester-diterpenoid alkaloids,monoester-diterpenoid alkaloids,and amine-diterpenoid alkaloids.Three pairs of isomers were detected and two of them were distinguished by the retention time of standard samples.Thirteen chemical markers were screened out through PCA and orthogonal partial least square discriminant analysis.Through detecting Napelline or isomer of Napelline(m/z 360.2530)and Aconifine(m/z 662.3170),AKRs from inner Mongolia autonomous could be screened.According to the existence of benzoylaconine(m/z 604.3108)and Indaconitine(m/z 630.3159),it could be confirmed that the AKRs are from Xinjiang Uygur autonomous.AKRs that cannot detect compounds above-mentioned could be from Liaoning or Shanxi Province.Conclusions:The chemical profile could be used not only to distinguish the AKRs from different geographic origins but also to identify the true and false of AKRs.This study lays a foundation for the study of efficacy and toxic of AKRs. 展开更多
关键词 Aconiti Kusnezoffii Radix chemical markers rapid differentiation ultra-performance liquid chromatography coupled with time-of-flight mass spectrometry
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梯度洗脱LC-ICP/MS法测定5种硒形态
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作者 陈思伊 唐琼 +2 位作者 黄丽 施向东 范云燕 《食品安全导刊》 2024年第13期100-103,共4页
建立一种梯度洗脱液相色谱-电感耦合等离子体质谱法(Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry,LC-ICP/MS)分析硒代胱氨酸、甲基硒代半胱氨酸、亚硒酸根、硒代蛋氨酸、硒酸根5种硒形态。样品通过Hamilton PR... 建立一种梯度洗脱液相色谱-电感耦合等离子体质谱法(Liquid Chromatography-Inductively Coupled Plasma-Mass Spectrometry,LC-ICP/MS)分析硒代胱氨酸、甲基硒代半胱氨酸、亚硒酸根、硒代蛋氨酸、硒酸根5种硒形态。样品通过Hamilton PRP-X100阴离子色谱柱,分别以流动相A 40 mmol·L^(-1)磷酸氢二铵+5 mmol·L^(-1)柠檬酸(pH=4.6)和流动相B 60 mmol·L^(-1)磷酸氢二铵+5 mmol·L^(-1)柠檬酸(pH=4.6)梯度洗脱5种硒形态,流速为1.0 mL·min^(-1),切换时间分别为3.0 min和6.4 min,ICP/MS检测,外标法定量。5种硒形态在8.5 min内检测完毕;0.5~200.0μg·L^(-1)相关系数r>0.999,最低检测质量浓度为0.10~0.39μg·L^(-1)。相较于《生活饮用水标准检验方法第6部分:金属和类金属指标》(GB/T 5750.6-2023)硒形态分析法,该方法将分析时间缩短了46.8%,5种形态峰分离度更好、灵敏度更高。 展开更多
关键词 硒形态 液相色谱-电感耦合等离子体质谱法 梯度洗脱
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清瘟护肺颗粒化学成分研究
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作者 龙凯花 刘静 +4 位作者 曹利平 刘满军 刘洋 杜霞 张红 《中国药业》 CAS 2024年第10期37-47,共11页
目的研究清瘟护肺颗粒的化学成分。方法查阅中国知网、PubMed、Web of Science等数据库,检索该制剂组方药材化学成分的相关文献,结合文献报道和ChemicalBook数据库信息,建立化学成分数据库。采用超高效液相色谱-四极杆/静电场轨道阱高... 目的研究清瘟护肺颗粒的化学成分。方法查阅中国知网、PubMed、Web of Science等数据库,检索该制剂组方药材化学成分的相关文献,结合文献报道和ChemicalBook数据库信息,建立化学成分数据库。采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q Exactive Focus MS/MS)法分析制剂的图谱数据,并以Xcalibur 4.0软件拟合分子式,与自建数据库信息进行匹配,初步推测分子式信息,与ChemicalBook或ChemSpider数据库比对,推测化学成分结构。结果共鉴定出158个化学成分,包括苷类36个,黄酮类29个,苯丙素类28个,有机酸类18个,萜类17个,色原酮类8个,其他类22个。结论所建立的方法可系统、准确、快速地定性分析清瘟护肺颗粒中的化学成分。 展开更多
关键词 清瘟护肺颗粒 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱法 化学成分 结构鉴定
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GLOBAL ANALYSIS OF THE METABOLITES OF CURCUMIN IN RATS BY ULTRA PERFORMANCE LIQUID CHROMATOGRAPHY COUPLED WITH QUADRUPOLE TIME OF-FLIGHT TANDEM MASS SPECTROMETRY
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作者 Feng Qiu Tianyi Qiu +2 位作者 Yang Yu Liqin Ding Xinchi Feng 《World Journal of Traditional Chinese Medicine》 2015年第4期100-101,共2页
Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism... Curcumin,a safe natural yellow pigment with a wide range of pharmacological activities,is used both in herbal drugs and as a food coloring agents.Studies have shown that curcumin would suffer from extensive metabolism in vivoand the predominant metabolic pathways are reduction and conjugation.In order to comprehensively study the metabolism and enrich the metabolic profile of cxurcumin in vivo,we carried out this research.A systematic method with highly sensitive UPLC-Q/TOF-MS was established to analyze different biological samples of rats after 展开更多
关键词 GLOBAL ANALYSIS OF THE METABOLITES OF CURCUMIN IN RATS BY ULTRA PERFORMANCE liquid chromatography coupled WITH QUADRUPOLE TIME OF-FLIGHT TANDEM mass SPECTROMETRY
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超高效液相色谱-四极杆/静电场轨道阱高分辨质谱探究4-HO-MiPT染毒斑马鱼脑部代谢组学变化
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作者 陈宇彬 于交远 +2 位作者 孟梁 刘猛 赵森 《质谱学报》 EI CAS CSCD 北大核心 2024年第5期699-711,共13页
为评价色胺类新精神活性物质4-羟基-N-甲基-N-异丙基色胺(4-HO-MiPT)对大脑的毒性效应,本实验以斑马鱼为模式生物进行自发活动行为记录分析,采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLCQ/Orbitrap HRMS)分析斑马鱼大脑长... 为评价色胺类新精神活性物质4-羟基-N-甲基-N-异丙基色胺(4-HO-MiPT)对大脑的毒性效应,本实验以斑马鱼为模式生物进行自发活动行为记录分析,采用超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLCQ/Orbitrap HRMS)分析斑马鱼大脑长期染毒后的代谢产物,并在转录水平上检测斑马鱼脑部目标基因的变化。结果表明,注射药物4-HO-MiPT后,斑马鱼运动速度明显减慢,运动范围明显缩小。从斑马鱼大脑检测出37种差异代谢产物,其中7种升高,30种降低,并导致6条代谢通路改变。脑部基因转录水平检测发现,4个神经系统的基因转录水平下降,对大脑细胞产生影响。本实验证明了4-HO-MiPT对斑马鱼大脑产生毒性效应,对神经系统、免疫功能造成损害并影响体内代谢,对斑马鱼行为产生明显的抑制效果,同时从4-HO-MiPT造成的内源性影响推测其可能致癌。 展开更多
关键词 4-羟基-N-甲基-N-异丙基色胺(4-HO-MiPT) 超高效液相色谱-四极杆/静电场轨道阱高分辨质谱(UHPLC-Q/Orbitrap HRMS) 斑马鱼 行为模型 代谢组学
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抗坏血酸-磷酸溶液超声提取-高效液相色谱-电感耦合等离子体质谱法快速测定土壤中6种砷形态的含量
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作者 杨丽婷 隆星星 +2 位作者 王艳萍 郭怀兰 张垚 《理化检验(化学分册)》 CAS CSCD 北大核心 2024年第8期770-774,共5页
为解决高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)测定土壤中6种砷形态含量时色谱分离时间长以及亚砷酸根[As(Ⅲ)]易转化成砷酸根[As(Ⅴ)]的问题,进行了题示研究。在0.1 g土壤样品中添加体积比1∶1的1.6 mol·L^(-1)磷酸溶... 为解决高效液相色谱-电感耦合等离子体质谱法(HPLC-ICP-MS)测定土壤中6种砷形态含量时色谱分离时间长以及亚砷酸根[As(Ⅲ)]易转化成砷酸根[As(Ⅴ)]的问题,进行了题示研究。在0.1 g土壤样品中添加体积比1∶1的1.6 mol·L^(-1)磷酸溶液和0.5 mol·L^(-1)抗坏血酸溶液的混合溶液10 mL,常温下超声提取6 h,用水稀释至50 mL,经0.22μm聚醚砜膜过滤,用HPLC-ICP-MS测定滤液中砷甜菜碱(AsB)、As(Ⅲ)、二甲基砷(DMA)、砷胆碱(AsC)、一甲基砷(MMA)和As(Ⅴ)等6种砷形态的含量。在色谱分析中,以Dionex IonPac AG7色谱柱(50 mm×4 mm,10μm)为分析柱和保护柱,不同体积比的3.5 mmol·L^(-1)碳酸铵溶液和100 mmol·L^(-1)碳酸铵溶液的混合溶液为流动相进行梯度洗脱。结果显示:6种砷形态的质量浓度均在一定范围内和峰面积呈线性关系,检出限(3S/N)为0.010~0.050μg·L^(-1);按照标准加入法进行回收试验,回收率为92.0%~110%,测定值的相对标准偏差(n=6)均小于5.0%。方法用于6个实际土壤样品的分析,检出了As(Ⅲ)和As(Ⅴ),检出量分别为0.07~0.15μg·g^(-1)和3.44~8.61μg·g^(-1)。 展开更多
关键词 抗坏血酸 高效液相色谱-电感耦合等离子体质谱法 形态分析 土壤
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采用高效液相色谱-高分辨质谱研究脂多糖诱导的兔炎症急性期模型代谢组学
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作者 陈金栋 王高雨 +2 位作者 陈俊苗 邱一凡 王文艳 《质谱学报》 EI CAS CSCD 北大核心 2024年第5期666-672,共7页
本研究对新西兰白兔低剂量递增给予脂多糖(lipopolysaccharide,LPS),诱导炎症急性反应期模型,收集给予LPS前、给予LPS 2天和7天后的尿液样本,采用超高效液相色谱-高分辨质谱(UPLC-HRMS)技术检测,并进行非靶向代谢组学分析。利用主成分分... 本研究对新西兰白兔低剂量递增给予脂多糖(lipopolysaccharide,LPS),诱导炎症急性反应期模型,收集给予LPS前、给予LPS 2天和7天后的尿液样本,采用超高效液相色谱-高分辨质谱(UPLC-HRMS)技术检测,并进行非靶向代谢组学分析。利用主成分分析(PCA)和偏最小二乘法判别分析(PLS-DA)法筛选差异代谢物,并通过KEGG数据库进行差异代谢通路分析。结果表明,给予LPS 2天和7天后,白兔尿液中的差异代谢物与给药前相比有显著差异,分别鉴定出41和161个差异代谢物,主要与类固醇激素生物合成通路显著相关(p<0.01)。炎症急性反应期发生了代谢紊乱,类固醇激素生物合成通路上调,这为炎症急性反应期有关靶标验证和疾病治疗提供了信息。 展开更多
关键词 代谢组学 脂多糖(LPS) 差异代谢物 类固醇激素 高效液相色谱-高分辨质谱(UPLC-HRMS)
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食品中一种新型非法添加物O-丙基伐地那非的快速筛查和定量测定 被引量:1
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作者 饶雅琨 王苑桃 +5 位作者 孙晓 王涛 董曼曼 李旸 李荣 张亚锋 《食品安全质量检测学报》 CAS 2024年第6期228-235,共8页
目的对在食品中发现的一种非法添加的新型磷酸二酯酶5型(phosphodiesterase type 5,PDE-5)抑制剂O-丙基伐地那非进行结构解析并建立定量测定方法。方法采用高效液相色谱-二极管阵列检测器法(high performance liquid chromatography-dio... 目的对在食品中发现的一种非法添加的新型磷酸二酯酶5型(phosphodiesterase type 5,PDE-5)抑制剂O-丙基伐地那非进行结构解析并建立定量测定方法。方法采用高效液相色谱-二极管阵列检测器法(high performance liquid chromatography-diode array detector,HPLC-DAD)发现了一种未知的新型伐地那非类似物,采用超高效液相色谱-四极杆-静电场轨道阱高分辨质谱法(ultra performance liquid chromatography-quadrupole/electrostatic field orbitrap high resolution mass spectrometry,UPLC-Q-Orbitrap HRMS)对其结构进行质谱解析,并依据解析的化学结构购买对照品,确定该物质为O-丙基伐地那非。采用超高效液相色谱-三重四极杆质谱法(ultra performance liquid chromatography-coupled triple quadrupole mass spectrometry,UPLC-MS/MS)建立典型食品中O-丙基伐地那非的定量测定方法。结果O-丙基伐地那非在0.50~50.25 ng/mL质量浓度范围内线性关系良好,相关系数(r)为0.9998,方法检出限(S/N=3)为0.02mg/kg,方法的定量限(S/N=10)为0.05mg/kg,在咖啡、压片糖果、保健酒基质中3个水平加样回收率分别为91.8%~93.9%、84.9%~87.3%和95.6%~103.0%,相对标准偏差均不大于4.6%。采用该方法对市场监管部门送检的93批样品进行测定,结果其中17批检出O-丙基伐地那非,其含量为28~359 mg/kg。结论所建立的方法快速、灵敏、准确,可用于O-丙基伐地那非的筛查和定量。本研究思路可给其他非法添加未知物的鉴定提供参考。 展开更多
关键词 超高效液相色谱-四极杆-静电场轨道阱质谱法 超高效液相色谱-三重四极杆质谱法 非法添加 O-丙基伐地那非 伐地那非衍生物
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微波灰化-高效液相色谱-电感耦合等离子体质谱(ICP-MS)法测定茶叶中的铬酸铅
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作者 刘欠 吴绮莉 潘春秀 《中国无机分析化学》 北大核心 2024年第3期267-275,共9页
为了准确测定茶叶中铬酸铅的含量,为市场监管提供判断依据,茶叶样品经微波灰化仪在500℃的条件下灰化50 min后,用0.25 mol/L的NaOH和0.14 mol/L的Na_(2)CO_(3)混合碱性提取液在90~95℃下不间断搅拌提取10 min,提取液经色谱柱分离后,用... 为了准确测定茶叶中铬酸铅的含量,为市场监管提供判断依据,茶叶样品经微波灰化仪在500℃的条件下灰化50 min后,用0.25 mol/L的NaOH和0.14 mol/L的Na_(2)CO_(3)混合碱性提取液在90~95℃下不间断搅拌提取10 min,提取液经色谱柱分离后,用电感耦合等离子体质谱(ICP-MS)法测定^(52)Cr,建立了微波灰化-高效液相色谱-电感耦合等离子体质谱仪测定茶叶中铬酸铅的方法。研究表明,方法在5.00~500μg/L线性良好,相关系数为0.9998,方法检出限低至2.5 mg/kg,三水平加标回收率为91.3%~95.3%,精密度在1.1%~2.0%。与电炉灼烧茶叶相比,微波灰化具有检出限低、精密度高、准确度良好等特性,能够满足茶叶中铬酸铅的测定。 展开更多
关键词 微波灰化 高效液相色谱-电感耦合等离子体质谱法 铬酸铅 茶叶
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车用气雾剂中VOCs检测方法的研究
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作者 李思 陈攀金 +1 位作者 田丁炜 杜振霞 《分析测试学报》 CAS CSCD 北大核心 2024年第4期630-636,共7页
为准确测量气雾剂产品中挥发性有机化合物(VOCs)的成分及含量,设计了特定装置将气雾剂中推进剂和非推进剂进行分离,利用采集袋收集气雾剂中的推进剂,通过液液萃取法对非推进剂中的VOCs进行提取。以所建立的气相色谱-质谱/氢火焰离子化... 为准确测量气雾剂产品中挥发性有机化合物(VOCs)的成分及含量,设计了特定装置将气雾剂中推进剂和非推进剂进行分离,利用采集袋收集气雾剂中的推进剂,通过液液萃取法对非推进剂中的VOCs进行提取。以所建立的气相色谱-质谱/氢火焰离子化检测器(GC-MS/FID)联用方法对样品进行分析,其中推进剂气体组分含量用归一化法进行测定,非推进剂的VOCs依据检出种类,选择8种VOCs建立标准曲线。各物质在对应质量浓度范围呈良好的线性关系,相关系数(r^(2))均大于0.99;检出限和定量下限分别为0.25~0.50 mg/L和0.50~1.00 mg/L;回收率为90.5%~105%,相对标准偏差(RSD)为1.8%~9.3%。应用建立的方法分析6种不同功能的气雾剂产品,并计算其臭氧生成潜势。结果表明,推进剂部分主要检出丙烷、丁烷、二甲醚,非推进剂部分检出苯系物、烷烃、环烷烃、单萜类、羧酸衍生物、醚类,其中苯系物和单萜类含量较高。该方法可为企业改进产品配方提供参考,也可为监管部门提供技术支持。 展开更多
关键词 液液萃取 气相色谱-质谱/氢火焰离子化检测器联用 气雾剂 VOCS
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