期刊文献+
共找到1,900篇文章
< 1 2 95 >
每页显示 20 50 100
Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry
1
作者 Lech RODZIEWICZ Jolanta MASLOWIECKA +1 位作者 Anna SADOWSKA Halina CAR 《色谱》 CAS CSCD 北大核心 2017年第10期1048-1054,共7页
Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC... Five thyreostats(TSs),namely tapazole,thiouracil,methylthiouracil,propylthiouracil,and phenylthiouracil,were determined in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry(UHPLC-MS/MS)in positive electrospray ionization mode.Extraction and clean-up were achieved using a ChemElut cartridge with tert-butyl methyl ether,without a derivatization step.Separation was achieved on an Acquity UPLC SS T3 column.The mobile phase was acetonitrile and water containing 0.2%(v/v)formic acid.The mass spectrometer was operated in multiple reaction monitoring mode.Urine samples were spiked with TS solution at levels corresponding to 5,10,15,and 20μg/L.The accuracy(internal standard corrected)ranged from 92%to 107%,with a repeatability precision(relative standard deviation,RSD)less than 15%for all five analytes.The RSDs within-laboratory reproducibility was less than 26%.The decision limits(CCα)and detection capabilities(CCβ)were obtained from a calibration curve and were in the ranges of 3.1-6.1μg/L and 4.0-7.4μg/L,respectively.The CCαand CCβvalues were below the recommended concentration,which was set at 10μg/L.The results show that the described method is suitable for the direct detection of TSs in bovine urine.This method can also be used to determine TSs in porcine urine. 展开更多
关键词 ultra-high performance liquid chromatography-tandem mass spectrometry (uhplc-ms/ms) thyreostats (TSs) URINE
下载PDF
Detection of 36 antibiotics in coastal waters using high performance liquid chromatography-tandem mass spectrometry 被引量:14
2
作者 那广水 顾佳 +4 位作者 葛林科 张蓬 王震 刘春阳 张琳 《Chinese Journal of Oceanology and Limnology》 SCIE CAS CSCD 2011年第5期1093-1102,共10页
Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more ... Among pharmaceuticals and personal care products released into the aquatic environment, antibiotics are of particular concern, because of their ubiquity and health effects. Although scientists have recently paid more attention to the threat of antibiotics to coastal ecosystems, researchers have often focused on relatively few antibiotics, because of the absence of suitable analytical methods. We have therefore developed a method for the rapid detection of 36 antibiotic residues in coastal waters, including tetracyclines (TCs), sulfanilamides (SAs), and quinolones (QLs). The method consists of solid-phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC-MS/MS) analysis, using electrospray ionization (ESI) in positive mode. The SPE was performed with Oasis HLB and Oasis MCX cartridges. Chromatographic separation on a Cr8 column was achieved using a binary eluent containing methanol and water with 0.1% formic acid. Typical recoveries of the analytes ranged from 67.4% to 109.3% at a fortification level of 100 ng/L. The precision of the method, calculated as relative standard deviation (RSD), was below 14.6% for all the compounds. The limits of detection (LODs) varied from 0.45 pg to 7.97 pg. The method was applied to detemaine the target analytes in coastal waters of the Yellow Sea in Liaoning, China. Among the tested antibiotics, 31 were found in coastal 'waters, with their concentrations between the LOD and 212.5 ng/L. These data indicate that this method is valid for analysis of antibiotics in coastal waters. The study first reports such a large number of antibiotics along the Yellow Sea coast of Liaoning, and should facilitate future comprehensive evaluation of antibiotics in coastal ecosystems 展开更多
关键词 ANTIBIOTICS high performance liquid chromatography-tandem mass spectrometry SOLID-PHASEEXTRACTION coastal waters
下载PDF
Simultaneous Determination of Bisphenols and Alkylphenols in Water by Solid Phase Extraction and Ultra Performance Liquid Chromatography-tandem Mass Spectrometry 被引量:4
3
作者 SHAN Xiao Mei SHEN Deng Hui +2 位作者 WANG Bing Shuang LU Bei Bei HUANG Fa Yuan 《Biomedical and Environmental Sciences》 SCIE CAS CSCD 2014年第6期471-474,共4页
To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry ... To establish an analytical method for determination of four bisphenols (BPA, BPB, BPF, and BPS) and two alkylphenols (4-n-OP, 4-n-NP) in water by ultra performance liquid chromatography- tandem mass spectrometry (UPLC/MS/MS). The water samples were extracted and condensed with solid-phase extraction (SPE) using C18 cartridges and eluted by acetonitrile. Separation was carried out with Acquity BEH C8 column and detection were performed by UPLC/MS/MS. Quantification was calculated by using the internal standard BPA-d16 and 4-n-NP-d8. The linear correlation coefficients of these compounds in the range of 1.0-100.0μg/L were all over 0.999. The minimum detectable concentrations were 0.75-1.0 ng/L, and the recoveries ranged from 87.0% to 106.9%. 展开更多
关键词 UPLC BPA Simultaneous Determination of Bisphenols and Alkylphenols in Water by Solid Phase Extraction and ultra performance liquid chromatography-tandem mass spectrometry mass
下载PDF
Determination of Steroid Hormone Residues in Fish Tissues Using Gel Permeation Chromatography and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry 被引量:3
4
作者 LI Peipei YAN Zhongyong +3 位作者 SUN Xiumei CHEN Si CHEN Yin ZHANG Xiaojun 《Journal of Ocean University of China》 SCIE CAS CSCD 2018年第5期1171-1177,共7页
A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 s... A highly sensitive method was developed for the simultaneous determination of 8 steroid hormones in high-fat fish tissues using ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).The 8 steroid hormones were extracted from the tissues with diethyl ether.Differing from other common purification methods,the extract solutions were cleaned by gel permeation chromatography(GPC) using ethyl acetate-cyclohexane solution(1:1,v/v) as the mobile phase.The separation of target compounds was carried out by a BEH C18 column and a gradient elution consisting of acetonitrile and 0.2% aqueous formic acid(v/v).The compounds were detected under the multiple reaction monitoring(MRM) mode and quantified with external standard method.This method was validated with respect to linearity,specificity,accuracy and precision.A linearity with correlation coefficient larger than 0.995 was achieved in the range of 0.5 to 50 ng m L^(-1).The average recoveries at the spiked levels of 1.0,5.0,and 10.0 μg kg^(–1) varied between 81.7% and 90.8%,with the relative standard deviations(n=5) ranged from 3.50% to 10.0%.The limit of quantification(LOQ) for 8 steroid hormones ranged from 0.2 to 1.5 μg kg^(-1).It was concluded that this method can be successfully applied for the determination of 8 steroid hormones in complicated matrices including high-fat fish tissues. 展开更多
关键词 ultra performance liquid chromatography-tandem mass spectrometry anabolic hormone gel permeation chromatography fish tissue
下载PDF
Chemical Components of Achyranthes bidentata Leaves by Ultra High Performance Liquid Chromatography-Mass Spectrometry 被引量:1
5
作者 Haiyang DONG Jinshuo MA Fulin YAN 《Medicinal Plant》 CAS 2019年第4期16-19,共4页
[Objectives] To study the chemical components and relative content of Achyranthes bidentata leaves and provide a scientific basis for further development and utilization of A. bidentata leaves.[Methods] The chemical c... [Objectives] To study the chemical components and relative content of Achyranthes bidentata leaves and provide a scientific basis for further development and utilization of A. bidentata leaves.[Methods] The chemical components of A. bidentata leaves were rapidly analyzed using the ultra high performance liquid chromatography-time of flight-high resolution mass spectrometry (UHPLC-TOF-MS).[Results] Thirty eight chemical compounds were identified in samples of A. bidentata leaves collected from Wen County of Henan Province, in which seven chemical compounds had the relative content higher than 5%, linoleic acid reached 25.7% and inokosterone A reached 13.8%.[Conclusions] A. bidentata leaves contain many kinds of chemical compounds. This study is expected to provide a certain basis for further extraction of linoleic acid and inokosterone A. 展开更多
关键词 Achyranthes bidentata LEAVES ultra high performance liquid chromatography-mass spectrometry (uhplc-ms) Chemical components Inokosterone
下载PDF
Simultaneous Determination of Ultraviolet Absorbers and Antibacterial Agents in Textiles by Ultra-High Performance Liquid Chromatography/Orbitrap High Resolution Mass Spectrometry 被引量:1
6
作者 Chengyun Wang Tangtang Xie +2 位作者 Rong Xu Junfeng Lin Lixia Li 《World Journal of Engineering and Technology》 2017年第1期1-18,共18页
This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile sampl... This paper reported a new analytical method for the simultaneous determination of seven benzotriazole ultraviolet absorbers and seven antibacterial agents in textiles. After ultrasonic extraction for the textile samples in methanol, the solutions were analyzed by ultra-high performance liquid chromotagraphy/orbitrap high resolution mass spectrometry (UPLC/Orbitrap HRMS). It showed that a good chromatographic separation for these target compounds was achieved by a Hypersil GOLD column (100 mm × 2.1 mm × 1.9 μm) with a gradient elution of methanol and 0.1% aqueous formic acid solution (containing 0.5 mmol/L ammonium acetate). Triclosan and 4-chloro-3,5-dimethyl phenol (PCMX) were detected by the orbitrap HRMS in an electrospray ionization (ESI) negative mode while the other twelve target compounds were detected by orbitrap HRMS in ESI positive mode. Full scan experiment was performed over the range from m/z 100 to m/z 500. These target compounds were routinely detected with mass accuracy below 2 × 10-6 (2 ppm) at the optimized conditions. The results showed that the limits of detection (LODs) were in the range from 0.1 to 0.3 μg/kg. The blank samples were spiked at three levels and their average recoveries varied from 80.5% to 96.3% while the relative standard deviation (RSD) changed from 3.2% to 9.9%. The present method was also applied for the determination of those ultraviolet absorbers and antibacterial agents in the commercial textiles. 展开更多
关键词 ultra-high performance liquid Chromatography/Orbitrap high Resolution mass spectrometry Benzotriazoleultraviolet ABSORBERS Isothiazolinone Tric-losan 4-Chloro-3 5-Dimethyl Phenol
下载PDF
Rapid Determination of Three Kinds of Microcystins in Environmental Water Samples by Disk SPE-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
7
作者 Zhao Bin Zhang Min Zhang Fuhai 《Meteorological and Environmental Research》 CAS 2016年第5期62-64,68,共4页
A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established.... A method of rapidly detecting three kinds of microcystins( MCs) in environmental water samples by using disk SPE- ultra high performance liquid chromatography- tandem mass spectrometry( UPLC- MS / MS) was established. Firstly,environmental water samples were extracted by disk SPE column( C_(18)),and three kinds of MCs were separated by Waters BEH C_(18) chromatographic column with acetonitrile- 0. 2% formic acid solution as the mobile phase. After the gradient elution separation,the external standard method was used for quantitative and qualitative analysis under MRM of UPLC- MS / MS. The results showed that the three kinds of MCs in the range of 0. 05- 10 μg / L showed good linear relation,and the correlation coefficients were higher than 0. 999 4,while the method detection limit was 0. 04 ng / L. Under 0. 1,1,and 5 μg / L standard addition for the same environmental sample,the average recovery was 82. 8%- 108. 8%,and the relative standard deviation of determination results was2. 1%- 10. 1%( n = 6). This method is rapid,sensitive and accurate,so it can be effectively applied in the monitoring of MCs in environmental water samples. 展开更多
关键词 Disk SOLID-PHASE extraction COLUMN ultra performance liquid chromatography-tandem mass spectrometry Environmental water sample MICROCYSTINS Lake Chao China
下载PDF
Simultaneous Determination of 14 β-Receptor Agonists Residues in Mutton by High Performance Liquid Chromatography-Tandem Mass Spectrometry (HPLC-MS/MS)
8
作者 Zhe MENG Jianhua WANG +5 位作者 Bo LIU Yuhang GUO Haoshuang DONG Pingyang SHAN Dawei WANG Yajuan SONG 《Agricultural Biotechnology》 CAS 2023年第5期55-58,共4页
[Objectives]A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of 14β-receptor agonist residues in mutton.[Methods]Samples were hydrolyzed byβ-g... [Objectives]A high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS)method was established for the determination of 14β-receptor agonist residues in mutton.[Methods]Samples were hydrolyzed byβ-glucuronidase and extracted with 5%acetic acid-acetonitrile(1:99,V/V)solution.An Eclipse plus C 18 column was used for separation,and the MRM mode was used for qualitative analysis,and the external standard method was used for quantitative analysis of matrix standard solutions.[Results]Under the optimal conditions,the retention time of the 14 kinds ofβ-receptor agonists ranged from 1.0 to 9.5 min.When the mass concentration was in the range of 0.05-0.50μg/ml,the linear relationship ofβ-receptor agonists was good,with correlation coefficients(r)≥0.9992.The detection limits of the method were in the range of 0.04-0.87μg/kg,and the quantitative limits were in the range of 0.35-1.86μg/kg.The average recovery values were in the range of 82.8%-108.9%,with RSDs(n=6)in the range of 1.9%-6.7%.[Conclusions]The method is simple,sensitive,reproducible,accurate,and can be used for simultaneous determination of the 14 kinds ofβ-receptor agonist residues in mutton. 展开更多
关键词 MUTTON high performance liquid chromatography-tandem mass spectrometry β-receptor agonist RESIDUE
下载PDF
Determination of okadaic acid related toxins from shellfish (<i>sinonovacula constricta</i>) by high performance liquid chromatography tandem mass spectrometry
9
作者 Hai-qi Zhang Weicheng Liu +3 位作者 Xin He Li-jun Liang Wenyong Ding Zhong-yang He 《Agricultural Sciences》 2013年第5期1-6,共6页
Consumption of shellfish contaminated with algal toxins produced by marine dinoflagellates can lead to diarrhetic shellfish poisoning (DSP). It was therefore essential that there are analytical techniques to identify ... Consumption of shellfish contaminated with algal toxins produced by marine dinoflagellates can lead to diarrhetic shellfish poisoning (DSP). It was therefore essential that there are analytical techniques to identify and quantify DSP toxins in shellfish. This new methodology could facilitate DSP monitoring and create a means of rapidly responding to incidents threatening public health. In the last years there were different analytical methods for DSP, such as mouse bioassay and LC-FLD. With the development of instrument, Liquid chromatography-mass spectrometry was substituted for other analytical methods with its good sensitivity and selectivity and without derivatization for the determination of DSP. In this report, a high performance liquid chromatogra-phytandem mass spectrometric(HPLC-MS/MS)method was developed for the simultaneous determination of okadaic acid (OA) and dinophysistoxins(DTX1) in Sinonovacula constricta. Optimization of pretreatment experiment was carried out to maximize recoveries and the effectiveness. The analytes were determined under multi-reactions monitoring (MRM) scan type with tandem mass analyzer using negative ion electrospray ionization (-ESI) mode .Finally, the detection and identification of OA and DTX-1 were based upon their retention times (RT) and the fragmentation patterns of their mass spectra. The method of LOQ for the two poisons was 0.02 mg·kg-1.The real sample test showed that this method could be used for sensitive, fast, and accurate determination of the two diarrheic shellfish poisons in shellfish. 展开更多
关键词 Sinonovacula Constricta high performance liquid chromatography-tandem mass spectrometry Okadaic Acid Dinophysistoxins-1
下载PDF
UHPLC-MS/MS测定睫毛类化妆品中14种前列腺素类似物含量
10
作者 陈安丽 张静 +2 位作者 曾敏珊 严小红 丁怡 《香料香精化妆品》 CAS 2024年第6期83-89,共7页
建立超高效液相色谱-串联三重四极杆质谱(UHPLC-MS/MS)法测定睫毛类化妆品中苯甲酸拉坦内酯、比马前列素、氯前列醇等14种前列腺素类似物。样品以四氢呋喃为分散剂,经乙腈提取、饱和氯化钠溶液除杂,离心、取上清液过滤后,采用Poroshell ... 建立超高效液相色谱-串联三重四极杆质谱(UHPLC-MS/MS)法测定睫毛类化妆品中苯甲酸拉坦内酯、比马前列素、氯前列醇等14种前列腺素类似物。样品以四氢呋喃为分散剂,经乙腈提取、饱和氯化钠溶液除杂,离心、取上清液过滤后,采用Poroshell 120 EC-C18柱(150 mm×3.0 mm×2.7μm)分离,以5 mmol/L甲酸铵(含质量分数0.1%甲酸)-乙腈为流动相,外标法定量。结果显示,14种前列腺素类似物在5~50 ng/mL线性关系良好,检出限(LOD)均在0.8μg/g内,定量限(LOQ)均在3μg/g以内。平均回收率为81.9%~119.7%,相对标准偏差(RSD)小于5%。该方法快速简便、灵敏准确,适用于睫毛类化妆品中14种前列腺素类似物的测定。 展开更多
关键词 睫毛 化妆品 前列腺素类似物 超高效液相色谱-串联三重四极杆质谱法
下载PDF
基于UHPLC-MS/MS法分析补肾利咽汤物质基准的特征图谱暨多指标成分的筛选与含量测定研究
11
作者 赵威 马永璠 +4 位作者 刘忠义 宋丽敏 刘艳华 张守琳 初洪波 《世界科学技术-中医药现代化》 CSCD 北大核心 2024年第3期704-720,共17页
目的采用超高效液相-质谱(UHPLC-MS/MS)法同时测定补肾利咽汤(BSLYT)中化学成分,建立BSLYT物质基准的高效液相色谱指纹图谱及莫诺苷、马钱苷、木蝴蝶苷A、木蝴蝶苷B、黄芩苷、落新妇苷等6种主要成分的含量测定方法,为质量控制提供参考... 目的采用超高效液相-质谱(UHPLC-MS/MS)法同时测定补肾利咽汤(BSLYT)中化学成分,建立BSLYT物质基准的高效液相色谱指纹图谱及莫诺苷、马钱苷、木蝴蝶苷A、木蝴蝶苷B、黄芩苷、落新妇苷等6种主要成分的含量测定方法,为质量控制提供参考。方法利用质谱数据,建立指纹图谱。用外标法计算BSLYT样品中主要成分的含量,并结合化学计量学方法分析不同批次样品的差异。结果质谱共指认出了69种化合物,经过与高效液相色谱比对,共指认出13种化合物。15批BSLYT物质基准特征图谱的相似度在0.90以上,共指认了27个共有峰。聚类分析(CA)将物质基准分为2类,即S1、S2、S5、S8、S9、S13、S15为一类,S3、S4、S6、S7、S10-S12、S16为一类。通过主成分分析(PCA)和正交偏最小二乘法判别分析(OPLSDA),筛选出影响物质基准分类的化学成分,分别归属于木蝴蝶、山茱萸和土茯苓。多指标成分含量测定6个成分,分别为莫诺苷、马钱苷、木蝴蝶苷A、木蝴蝶苷B、黄芩苷、落新妇苷含量范围分别在0.31%-0.51%、0.12%-0.22%、0.09%-0.19%、0.09%-0.24%、0.07%-0.18%、0.08%-0.29%。结论本文建立的指纹图谱和多指标含量测定方法准确、稳定,为补肾利咽汤的物质基准及相关制剂的质量控制提供依据。 展开更多
关键词 补肾利咽汤 物质基准 超高效液相-质谱 指纹图谱 含量测定 化学计量学
下载PDF
Determination of chlorpromazine in porcine muscle using high performance liquid chromatography-tandem mass spectrometry
12
作者 张露 黄雯 蒋心惠 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2015年第10期690-694,共5页
A rapid and accurate high performance liquid chromatography tandem mass spectrometry(HPLS-MS) method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitril... A rapid and accurate high performance liquid chromatography tandem mass spectrometry(HPLS-MS) method was established for quantification of chlorpromazine in pork. The porcine samples were pretreated with acetonitrile to precipitate proteins and followed by extraction with tert--butyl methyl ether(TBME). The separation was performed on a 5 μm Agilent XDB--C18 column with gradient elution. The mobile phase A was 0.01 mol/L ammonium formate in water and mobile phase B was acetonitrile. The flow rate was at 0.8 mL/min. Quantification was performed on a triple-quadrupole tandem mass spectrometer using the multiple selected reaction monitoring(MRM) mode. Transition of m/z +319.1 to 58.1 was used for the quantification of chlorpromazine. The method was validated at the concentration range of 0.4040 μg/kg to 8.080 μg/kg for chlorpromazine with correlation coefficient of 0.9999. The spiked recoveries were more than 80.0% and the limit of detection(LOD) was 0.052 μg/kg. The developed method, which offers advantages of convenience, rapid, specificity and higher sensitivity, can be used for determination of chlorpromazine hydrochloride in porcine muscles. 展开更多
关键词 high performance liquid chromatography-tandem mass spectrometry Chlorpromazine hydrochloride Porcine muscle Residual quantification
原文传递
UHPLC-MS/MS法测定大鼠血浆中环磷酰胺及其代谢物的浓度 被引量:8
13
作者 陈力 熊筱娟 +5 位作者 高守红 翟健秀 陈万生 刘震 黄宏伟 张凤 《第二军医大学学报》 CAS CSCD 北大核心 2016年第9期1063-1069,共7页
目的建立利用超高效液相色谱-串联质谱(UHPLC-MS/MS)法同时测定大鼠血浆中环磷酰胺及其代谢产物(羧基磷酰胺、4-酮基环磷酰胺和脱氯乙基环磷酰胺)浓度的方法。方法以Agilent poroshell SB-C_(18)柱(75mm×2.1mm,2.7μm)为色谱柱,甲... 目的建立利用超高效液相色谱-串联质谱(UHPLC-MS/MS)法同时测定大鼠血浆中环磷酰胺及其代谢产物(羧基磷酰胺、4-酮基环磷酰胺和脱氯乙基环磷酰胺)浓度的方法。方法以Agilent poroshell SB-C_(18)柱(75mm×2.1mm,2.7μm)为色谱柱,甲醇-10mmol/L乙酸铵溶液为流动相进行梯度洗脱,流速0.25mL/min,柱温25℃,进样量5μL;质谱采用电喷雾离子源(ESI),选择多重反应离子监测(MRM)正离子模式。取8只成年雄性SD大鼠分离获得血浆样品,测定血浆样品中环磷酰胺及其代谢产物的血药浓度和药代动力学参数。结果方法学验证表明,环磷酰胺、羧基磷酰胺、4-酮基环磷酰胺在浓度为20~4 000ng/mL范围内线性关系良好(r分别为0.998 0、0.995 3和0.998 6),脱氯乙基环磷酰胺在浓度为5~1 000ng/mL范围内线性关系良好(r=0.996 8)。日内、日间相对标准差(RSD)对于质控(QC)样品和最低定量限(LLOQ)样品分别小于8.73%和15.38%,基质因子的RSD均在-15%~15%之间,提取回收率均在(66.44±5.53)%^(96.66±1.73)%之间;所有待测化合物的稳定性均表现良好。大鼠血浆中各化合物药代动力学参数如下:环磷酰胺、羧基磷酰胺、4-酮基环磷酰胺和脱氯乙基环磷酰胺的Cmax分别为(207.52±13.20)、(18.47±2.66)、(6.59±1.33)和(8.27±1.44)μg/mL,T_(1/2)分别为(1.28±0.09)、(5.03±0.48)、(6.72±0.47)和(7.47±0.68)h,AUC_(0→t)分别为(372.52±32.79)、(65.70±5.04)、(33.26±11.76)和(45.03±8.93)μg·h·mL^(-1)。结论该方法操作简单、灵敏、准确、专属性强,适用于高剂量环磷酸铵在大鼠血浆中药代动力学研究。 展开更多
关键词 环磷酰胺 代谢 超高效液相色谱-串联质谱法 药代动力学
下载PDF
用UHPLC-MS/MS法同时测定肾八味胶囊中6种皂苷的含量
14
作者 杨宇 周灿灿 唐跃年 《药学服务与研究》 CAS 2016年第6期452-456,共5页
目的:建立超高效液相联用质谱法(UHPLC—MS/MS)同时测定肾八味胶囊中6种皂苷(人参皂苷Rb1、三七皂苷R1、人参皂苷Rg1、人参皂苷F1、人参皂苷F2、原人参三醇)的含量。方法:采用Zorbax SB-C18色谱柱(2.1mm×50mm,1.8μm)... 目的:建立超高效液相联用质谱法(UHPLC—MS/MS)同时测定肾八味胶囊中6种皂苷(人参皂苷Rb1、三七皂苷R1、人参皂苷Rg1、人参皂苷F1、人参皂苷F2、原人参三醇)的含量。方法:采用Zorbax SB-C18色谱柱(2.1mm×50mm,1.8μm),以0.1%甲酸水溶液(A相)-0.1%甲酸乙腈溶液(B相)为流动相梯度洗脱(0~3.2min,20%~35%B相;3.2~3.4min,25%~45%B相;3.4~7.0min,45%~55%B相),流速为0.3ml/min,柱温20℃,进样量5μl,采用电喷雾离子源(ESI)正离子模式下检测。结果:人参皂苷Rb1、三七皂苷R1、人参皂苷Rg1、人参皂苷F1、人参皂苷F2和原人参三醇在相应的线性范围内线性关系良好(r≥0.9991),日内和日间RSD为0.54%~2.92%,平均加样回收率为97.06%~99.76%,重复性和稳定性良好。结论:本研究建立的UHPLC-MS/MS法能够快速、简便、灵敏地测定肾八味胶囊中6种皂苷的含量。主成分分析(PCA)和偏最小二乘判别分析(PLS-DA)可对有效期不同的样品进行区分,由此可为肾八味胶囊的质量控制提供科学依据。 展开更多
关键词 肾八味胶囊 皂苷类 含量测定 色谱法 超高效液相 质谱法 联用
下载PDF
UHPLC-MS/MS快速检测人体血清中的2种抗精神病药物 被引量:2
15
作者 刘云 王裕锋 +3 位作者 蒋家兵 闫小华 林才勇 詹松 《中南药学》 CAS 2017年第6期811-814,共4页
目的建立超高效液相色谱和三重四极杆质谱联用快速测定人体血清中2种抗精神病药物的分析方法。方法空白人血清加标后用0.22μm尼龙滤膜过滤,直接加纯水稀释10倍后,用超高效液相色谱分离,三重四极杆质谱进行定量分析。结果 2种药物在1~20... 目的建立超高效液相色谱和三重四极杆质谱联用快速测定人体血清中2种抗精神病药物的分析方法。方法空白人血清加标后用0.22μm尼龙滤膜过滤,直接加纯水稀释10倍后,用超高效液相色谱分离,三重四极杆质谱进行定量分析。结果 2种药物在1~200μg·L^(-1)与峰面积呈良好的线性关系,r均>0.9998,不同浓度下加样回收率在70.1%~116.8%,定量限在0.25~0.29μg·L^(-1)。结论该方法简便、高效、快速、高灵敏度,可用于药代动力学研究及临床血药浓度监测。 展开更多
关键词 血清 抗精神病药物 超高效液相色谱法 三重四极杆质谱仪
下载PDF
UHPLC-MS/MS法同时测定热毒宁注射液中5种成分 被引量:2
16
作者 王超众 南俊伶 +1 位作者 董艳丽 王萌萌 《中成药》 CAS CSCD 北大核心 2022年第10期3126-3130,共5页
目的 建立超高效液相色谱-三重四级杆串联质谱(UHPLC-MS/MS)法同时测定热毒宁注射液(金银花、栀子、青蒿)中栀子苷、京尼平龙胆双糖苷、绿原酸、新绿原酸、隐绿原酸的含量。方法 该药物50%甲醇提取液的分析采用ACES CDim色谱柱(100 mm&#... 目的 建立超高效液相色谱-三重四级杆串联质谱(UHPLC-MS/MS)法同时测定热毒宁注射液(金银花、栀子、青蒿)中栀子苷、京尼平龙胆双糖苷、绿原酸、新绿原酸、隐绿原酸的含量。方法 该药物50%甲醇提取液的分析采用ACES CDim色谱柱(100 mm×2.1 mm, 1.7μm);流动相乙腈-5 mmol/L甲酸铵(含0.1%甲酸),梯度洗脱;体积流量0.3 mL/min;柱温30℃;电喷雾离子源,正负离子检测,选择反应监测模式。结果 5种成分在各自范围内线性关系良好(r>0.999 4),平均加样回收率98.88%~99.99%,RSD 1.21%~2.10%。结论 该方法快速、简便、准确,可用于热毒宁注射液的质量控制。 展开更多
关键词 热毒宁注射液 化学成分 超高效液相色谱-三重四级杆串联质谱(uhplc-ms/ms)
下载PDF
UHPLC-MS/MS法检测中成药及保健食品中非法添加文拉法辛的研究 被引量:2
17
作者 王超众 王萌萌 +5 位作者 刘信奎 张连成 于百青 杨敏 孙伟 初红涛 《中国实用医药》 2021年第10期207-209,共3页
目的探讨超高效液相色谱-串联质谱法(UHPLC-MS/MS法)检测中成药及保健食品中非法添加文拉法辛的应用价值。方法采用超高效液相色谱-串联质谱法,离子源为电喷雾电离源(ESI源),正离子模式检测中成药及保健食品中非法添加的文拉法辛浓度。... 目的探讨超高效液相色谱-串联质谱法(UHPLC-MS/MS法)检测中成药及保健食品中非法添加文拉法辛的应用价值。方法采用超高效液相色谱-串联质谱法,离子源为电喷雾电离源(ESI源),正离子模式检测中成药及保健食品中非法添加的文拉法辛浓度。结果文拉法辛在50~2000 ng/ml的浓度范围内呈良好的线性关系(r=0.9998),方法检出限(LOD)为0.35μg/g,加样回收率为98.59%,相对标准偏差为1.63%。结论采用超高效液相色谱-串联质谱法对中成药及保健食品中非法添加文拉法辛的浓度进行检测,其简便、准确、灵敏度高,可作为分析中成药及保健食品中非法添加文拉法辛的有效检测方法。 展开更多
关键词 超高效液相色谱-串联质谱法 中成药 保健食品 文拉法辛 非法添加
下载PDF
氨基类神经递质的N-乙基化法UHPLC-MS/MS定量分析技术 被引量:2
18
作者 薛海斯 唐惠儒 《上海交通大学学报(医学版)》 CAS CSCD 北大核心 2018年第11期1300-1305,共6页
目的·为了研究氨基类神经递质的含量变化对生物体的生理及病理生理过程的影响,探讨这类代谢物的高灵敏定量分析方法。方法·使用乙醛与氰基硼氢化钠(NaBH_3CN)的一对稳定同位素标记试剂分别对氨基类神经递质进行N-乙基化柱前衍... 目的·为了研究氨基类神经递质的含量变化对生物体的生理及病理生理过程的影响,探讨这类代谢物的高灵敏定量分析方法。方法·使用乙醛与氰基硼氢化钠(NaBH_3CN)的一对稳定同位素标记试剂分别对氨基类神经递质进行N-乙基化柱前衍生,采用超高效液相色谱-串联质谱联用技术(ultra-high performance liquid chromatography-tandem mass spectrometry,UHPLC-MS/MS),对20种氨基类神经递质进行一次性高灵敏内标定量分析。结果·方法学验证表明该20种氨基类神经递质均呈现良好的线性关系(相关系数R^2>0.991 0);除组胺检测限为36.5 fmol外,其余物质均在0.5~10 fmol范围;日间差及日内差的相对标准偏差低于15%。使用该方法对人尿液、血清及唾液样本中的氨基类神经递质进行定量检测分析,分别可检测到14、10及8种神经递质。结论·该方法具有较高检测灵敏度及精密度,可用于人尿液、血清及唾液样本中神经递质的定量分析;与已有方法相比,此方法具有反应条件温和、操作简便、反应原料易于淬灭、灵敏度与精密度高等优势,可实现多种氨基类神经递质的一次性高灵敏定量分析。 展开更多
关键词 氨基 神经递质 N-乙基化柱前衍生 超高效液相色谱-串联质谱联用技术 定量分析
下载PDF
基于UHPLC-MS/MS法,中毒量氯化琥珀胆碱在大鼠体内分布的研究
19
作者 盛洁 姜荣 +8 位作者 文继月 陈林 解启文 方俊杰 万阳 秦明 李婧 陈冠军 陈志武 《中国药理学通报》 CAS CSCD 北大核心 2020年第5期670-675,共6页
目的建立适当的超高效液相色谱串联质谱(UHPLC-MS/MS)法,测定中毒量氯化琥珀胆碱(succinylcholine chloride,Suc)在大鼠体内的分布。方法大鼠分别皮下注射3种剂量的Suc,4 h后取大鼠血清和各主要脏器组织进行乙腈蛋白沉淀并过固相萃取WC... 目的建立适当的超高效液相色谱串联质谱(UHPLC-MS/MS)法,测定中毒量氯化琥珀胆碱(succinylcholine chloride,Suc)在大鼠体内的分布。方法大鼠分别皮下注射3种剂量的Suc,4 h后取大鼠血清和各主要脏器组织进行乙腈蛋白沉淀并过固相萃取WCX柱进行纯化;色谱采用Luna NH2色谱柱(2 mm×100 mm,3μm),流动相为0.1%甲酸水溶液-乙腈等度洗脱,质谱测定采用正离子扫描下多反应监测模式(MRM)。对Suc离子对(m/z 145.1→93.3,m/z 145.1→115.4)进行定性、定量分析。结果Suc的检测限是0.01μg·L^-1,回收率为89.5%~95.4%,日内、日间RSD均小于15%。除NS对照组外,3种剂量的Suc组大鼠的血清及心、肝、肾等主要脏器组织中均检测到Suc,并且肾组织中的Suc最高。结论大鼠Suc中毒时在血清及心、肝、肾等组织中均有分布,其中肾脏中含量最高;UHPLC-MS/MS法是检测Suc中毒大鼠体内药量的一个有效、可靠的方法。 展开更多
关键词 超高效液相色谱串联质谱法 氯化琥珀胆碱 大鼠 血清 固相萃取 肾脏
下载PDF
QuEChERS结合UHPLC-MS/MS法测定畜肉中阿苯达唑及其代谢物的残留量 被引量:5
20
作者 黄永桥 杨昌彪 +2 位作者 马凯 毛敏霞 简银池 《食品与发酵工业》 CAS CSCD 北大核心 2021年第19期258-263,共6页
该文建立了快速测定畜肉中阿苯达唑及其代谢物(阿苯达唑砜、阿苯达唑亚砜、阿苯达唑-2-氨基砜)残留量的超高效液相色谱-串联质谱的分析方法。试样用乙腈提取,经QuEChERS试剂净化,通过Agilent ZORBAX Eclipse Plus C 18色谱柱分离,在正... 该文建立了快速测定畜肉中阿苯达唑及其代谢物(阿苯达唑砜、阿苯达唑亚砜、阿苯达唑-2-氨基砜)残留量的超高效液相色谱-串联质谱的分析方法。试样用乙腈提取,经QuEChERS试剂净化,通过Agilent ZORBAX Eclipse Plus C 18色谱柱分离,在正离子多反应监测模式下分析,外标法定量。实验结果表明,阿苯达唑及其代谢物在各自的线性范围内线性关系良好(R ^(2)>0.998),检出限0.1~1μg/kg,在空白样品中进行3个浓度水平的添加实验,添加范围为0.1~10μg/kg,日内(n=6)平均回收率在81.9%~109.8%,日间(n=3)平均回收率在81.8%~99.0%,精密度为1.8%~14.4%。该方法操作简单、快速、准确、灵敏度高,重现性好,回收率高且稳定,检测限及定量限低于现有检测方法要求,可用于畜肉中阿苯达唑及其代谢物残留量的定性和定量分析。 展开更多
关键词 QUECHERS 超高效液相色谱-串联质谱法 畜肉 阿苯达唑及其代谢物
下载PDF
上一页 1 2 95 下一页 到第
使用帮助 返回顶部