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Determination of Oleuropein in Cosmetics by Ultra Performance Liquid Chromatography-Triple Quadrupole Tandem Mass Spectrometry
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作者 Pan Lijing Chen Weiwei Yuan Minjia 《China Detergent & Cosmetics》 CAS 2023年第4期30-36,共7页
An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracte... An ultrahigh performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS)was established to quickly and accurately determine the content of oleuropein in cosmetics.The samples were extracted with methanol-aqueous solution,and the mobile phase with methanol-formic acid solution(0.1 mol/L)=40∶60 was separated by Agilent ZORBAX Eclipse Plus C18(2.1 mm×50 mm×1.8μm-Micron)column temperature 30℃,flow rate 0.3 mL/min.The MS end was detected by electrospray negative mode ionization(ESI-)and multiple reaction monitoring(MRM)mode.The results show a good linear relationship in the range of 0.002~5 mg/L,with a correlation coefficient R2 of 0.999,5.Method recovery range from 84.2%~107.6%and the relative standard deviation RSD is 5.8%.The detection time is 5 min,the detection limit is 0.000,6 mg/L,and the limit of quantification is 0.002 mg/L.This method has the advantages of convenient operation,low quantification limit,high precision and good repeatability,and is suitable for measuring the content of oleuropein in many kinds of cosmetics. 展开更多
关键词 ultra performance liquid chromatography-triple quadrupole tandem mass spectrometry(UPLC-MS/MS) OLEUROPEIN COSMETICS
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Determination of thyreostats in bovine urine using ultra-high performance liquid chromatography-tandem mass spectrometry
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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
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Detection of 36 antibiotics in coastal waters using high performance liquid chromatography-tandem mass spectrometry 被引量:13
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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 C18 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 determine 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 抗生素残留 高效液相色谱 沿海水域 质谱检测 串联质谱 LC-MS/MS 沿海生态系统 个人护理产品
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Determination of Steroid Hormone Residues in Fish Tissues Using Gel Permeation Chromatography and Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry 被引量:3
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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 荷尔蒙 类固醇 脚踏车 层析 纸巾 液体 浸透 胶化
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Uncertainty Evaluation of Determination of Microcystin MC-LR in Environmental Samples by Solid Phase Extraction-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry 被引量:1
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作者 Zhao Bin Zhang Min Zhang Fuhai 《Meteorological and Environmental Research》 CAS 2016年第6期54-57,共4页
To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated first... To assess uncertainty of determination of MC-LR in environmental samples by solid phase extraction- ultra performance liquid chromatography- tandem mass spectrometry,the sources of the uncertainty were evaluated firstly,and the expanded uncertainty was calculated finally.The results show that when MC-LR concentration in the water samples was 0.50 μg/L,the expanded uncertainty was 0.00628 μg/L(k=2). 展开更多
关键词 UNCERTAINTY Solid phase extraction ultra performance liquid CHROMATOGRAPHY tandem mass spectrometry MICROCYSTIN MC-LR China
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Chemical Components of Achyranthes bidentata Leaves by Ultra High Performance Liquid Chromatography-Mass Spectrometry 被引量:1
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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
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Rapid Determination of Three Kinds of Microcystins in Environmental Water Samples by Disk SPE-Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
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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
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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
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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
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Modernization of Chinese herbal compound and the high performance liquid chromatography tandem mass spectrometry (HPLC-MS)
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作者 LI Wen-lan1,2,3,SUN Zhi1,2,DU Juan1,2(1.Engineering Research Center of natural antineoplastic drugs,Ministry of Education,Harbin 150076,China 2.Center of Research and Development on Life Sciences and Environmental Sciences,Harbin University of Commerce,Harbin 150076,China 3.Institute of Materia Medica and Postdoctoral Programme of Harbin University of Commerce,Harbin 150076,China) 《沈阳药科大学学报》 CAS CSCD 北大核心 2008年第S1期119-119,共1页
Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is ... Chinese herbal compound is playing an important role on curing human diseases.And it has been a trend that Chinese herbal compound is being used all over the world in 21 century.However,our Chinese herbal compound is facing serious challenge for the lack of canonical system of quality criterion for Chinese herbal compound so it has been a urgent problem to set up the quality control standards and reveal therapeutic basis of Chinese herbal compound.In order to give full play to the advantages of Chinese herbal compound,modern scientific and technological is used to research of Chinese herbal compound,especially the high performance liquid chromatography tandem mass spectrometry(HPLC-MS),because it is high sensitive,rapid,and obtain more information.It is very necessary that HPLC-MS is uesed to elucidate the effective components of basic substances of Chinese Herbal Compound,and endow traditional Chinese medicine with modern scientific connotation. 展开更多
关键词 MODERNIZATION of Chinese HERBAL compound the high performance liquid chromatography tandem mass spectrometry(HPLC-MS)
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Determination of okadaic acid related toxins from shellfish (<i>sinonovacula constricta</i>) by high performance liquid chromatography tandem mass spectrometry
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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
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Determination of 24 Allergens in Perfume with High Performance Liquid Chromatography Tandem Mass Spectrometry
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作者 Wang Yujian Liang Zhengang +1 位作者 Fu Lingmei Dong Cunzhu 《China Detergent & Cosmetics》 2019年第1期40-46,共7页
A method of 24 allergens determination in cosmetics were established with high performance liquid chromatography tandem mass spectrometry. The targeted compounds were extracted with acetonitrile and determined with LC... A method of 24 allergens determination in cosmetics were established with high performance liquid chromatography tandem mass spectrometry. The targeted compounds were extracted with acetonitrile and determined with LC-MS/MS (MRM mode) with external method. The linearity between concentrations and peak area ratio was obtained from 1.0~5.0 mg/L. The limits of detection were 1.0 mg/L for the instrument and 5.0 mg/kg for the method respectively. The LOQ was 15.0 mg/L. The average recoveries of 24 allergens were between 85.9% and 110.0% at spiked levels of 5, 10 and 20 mg/kg with relative standard derivation (RSDs) of 5.5%~12.0%(n=10). The method could be used as a reliable means for simultaneous quantitative determination of allergens in cosmetics. 展开更多
关键词 PERFUME allergens FLAVOR high performance liquid CHROMATOGRAPHY tandem mass spectrometry
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Detecting N-nitrosamines in water treatment plants and distribution systems in China using ultra-performance liquid chromatography-tandem mass spectrometry 被引量:11
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作者 Chengkun WANG Xiaojian ZHANG +1 位作者 Jun WANG Chao CHEN 《Frontiers of Environmental Science & Engineering》 SCIE EI CAS CSCD 2012年第6期770-777,共8页
N-nitrosodimethylamine (NDMA) and several other N-nitrosamines have been detected as disinfection by-products in drinking waters in many countries around the world. An ultra-performance liquid chromatography- tandem... N-nitrosodimethylamine (NDMA) and several other N-nitrosamines have been detected as disinfection by-products in drinking waters in many countries around the world. An ultra-performance liquid chromatography- tandem mass spectrometry method with solid phase extraction sample preparation was developed to study the occurrence of N-nitrosamines in several water treatment plants and distribution systems in China. Isotope labeled N-nitrosodi-n-propylamine-dl4 (NDPA-dl4) was selected as the internal standard for quantification. The solid phase extraction procedures including pH, enrichment process and MS/MS parameters including capillary voltage, cone gas flow, cone voltage, collision energy were optimized to give average recoveries of 26% to 112% for nine N- nitrosamine species. The instrument detection limits were estimated to range from 0.5 to 5μg.L-1 for the nine N- nitrosamine species. NDMA and several other N-nitrosa- mines were found at fairly high concentrations in several water treatment plants and distribution systems. NDMA was found in all locations, and the highest concentrations in cities B, G, T, and W were 3.0, 35.7, 21.3, and 19.7 ng. L 1, respectively. A wide range of N-nitrosamines concentrations and species were observed in different locations. Higher concentrations of N-nitrosamines were detected in distribution systems that were further away from the treatment plants, suggesting that the contact time between the residual disinfectant and natural organic matter may play an important role in the formation of these compounds. 展开更多
关键词 N-NITROSAMINES water treatment plant distri-bution system ultra-performance liquid chromatography-tandem mass spectrometry
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Development of a Rapid and Simultaneous Detection Method for Buprenorphine, Norbuprenorphine and Naloxone in Human Plasma Using Ultra-high Performance Liquid Chromatography- tandem Mass Spectrometer with Solid-phase Extraction 被引量:1
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作者 Guo, Qiaozhen Du, Zhenxia 《Chinese Journal of Chemistry》 SCIE CAS CSCD 2011年第9期1922-1926,共5页
A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine (BP), its primary metabolite, nor-buprenorphine (NBP) and a proposed co-formulate, naloxone ... A simultaneous method was successfully established and validated for the separation and determination of bu- prenorphine (BP), its primary metabolite, nor-buprenorphine (NBP) and a proposed co-formulate, naloxone (NLX) in human plasma. The method used buprenorphine-d4 (BP-D4), nor-buprenorphine-d3 (NBP-D3), naltrexone (NTX) as internal standards (ISs). 100 μL of plasma sample fortified with the ISs was cleaned up by solid-phase extraction (SPE), and was then separated on a Waters AcquityTM BEH C18 column with gradient elution using methanol and water (containing 0.2% formic) at a flow rate of 0.25 mL·min^-1. The mass spectrometer was used for detection and was operated in the positive electrospray ionization with multiple reaction monitoring (MRM) mode. The three compounds were effectively separated in 5 min. The linear ranges of the compounds were 0.1--25, 0.25--25 and 0.05--25 ng·mL^-1 for BP, NBP and NLX, respectively, with r≥0.9935. The method had high sensitivity (the lim- its of detection were 0.02, 0.1 and 0.01 ng.mL-1 for BP, NBP and NLX, respectively) and high recoveries (≥97.6%). The result was shown to be linear and satisfactorily met current acceptance criteria for validation of bio- analytical method: intra and inter assay precisions within the required limits of ≤25% RSD. The LOQs fulfilled the LOQ requirements: precision≤25% RSD, and was fully validated according to the State Food and Drug Administration (SFDA) regulations. The results demonstrated that ultra-high performance liquid chromatography- tandem mass spectrometer (UPLC-MS/MS) with SPE was a powerful detection tool and contributed to pharmaceutical analysis in biological matrices. 展开更多
关键词 ultra-high performance liquid chromatography-tandem mass spectrometer BUPRENORPHINE naloxone norbuprenorphine human plasma
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Rapid Determination of Tetrodotoxin in Human Plasma by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry
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作者 CHEN Weizhu ZHANG Yiping +3 位作者 SUN Jipeng XIE Quanling HONG Zhuan YI Ruizao 《Chemical Research in Chinese Universities》 SCIE CAS CSCD 2018年第6期905-911,共7页
A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tande... A sensitive analytical method was developed to determine tetrodotoxin(TTX) in human plasma samples using protein precipitation, followed by ultra performance liquid chromatography(UPLC) analysis coupled with tandem mass spectrometry(MS/MS) using 11-deoxytetrodotoxin(11-deoxyTTX) as an internal standard. The plasma samples were prepared using protein precipitation prior to being analyzed by UPLC-MSfMS to identify TTX over a zwitterionic-hydrophilic interaction liquid chromatography column. The retention time values of TTX and 11-deoxyTTX were 4.12 and 3.67 min, respectively. TTX and 11-deoxyTTX were monitored and quantitated on the basis of their ion transitions for their respective precursor ions to their product ions(i.e., m/z 320.0→162. l for TTX and m/z 304.0→176.0 for 11-deoxyTTX) in the multiple reaction-monitoring mode. The lower limit of quantification of this method was determined to be 0.0199 ug/mL. This method showed good linearity for plasma samples that contained TTX concentrations in the range of 0.0199--1.99 ng/mL. The specificity, precision, accuracy, matrix effect, and stability characteristics of this method were also examined. The intra-assay precision and accuracy ranged from 1.89% to 6.00% and from 92.21% to 100.00%, whereas the inter-assay precision and accuracy ranged from 0.64% to 7.75% and from 99.38% to 101.26%, respectively. This new method therefore represents a rapid, accurate, reliable, and highly sensitive method for the qualitative and quantitative analyses of a trace amount of TTX in human plasma samples. 展开更多
关键词 Tetrodotoxin(TTX) 11-DeoxyTTX ultra performance liquid chromatography(UPLC)coupled with tandem mass spectrometry(MS/MS) PLASMA Protein precipitation
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Simultaneous Determination of Six Compounds in Rat Plasma by Ultra-Performance Liquid Chromatography with Tandem Mass Spectrometry: Application in the Pharmacokinetic Study of Qing Gan-Shu Yu-Fang 被引量:1
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作者 Hai Jiang A-Jiao Houa +10 位作者 Yan-Yan Zhang Wen-Jing Man Liu Yang Yong-Hai Meng Xin-Yue Guo Song Wang Jia-Xu Zhang Bing-You Yang Qiu-Hong Wang Kelvin Chan Hai-Xue Kuang 《World Journal of Traditional Chinese Medicine》 2019年第4期250-259,共10页
A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,s... A rapid and high selective ultra-performance liquid chromatography(UPLC)with tandem mass spectrometry method for simultaneous determination of six compounds including albiflorin,paeoniflorin,picroside I,picroside II,saikosaponin A,and saikosaponin D in rat plasma was developed and validated using butyl p-hydroxybenzoate as an internal standard.One-step direct protein precipitation with acetonitrile was used to extract the compounds from the rat plasma samples.Chromatographic separation was achieved using an ACQUITY UPLC BEH C18 column(100 mm×2.1 mm,1.7μm)at a flow rate of 0.4 m L/min,using gradient mode containing 0.1%formic acid in water and acetonitrile were used as the Mobile phase A and B.Electrospray ionization in negative ion mode and multiple reaction monitoring were used to identify and quantify active components.Calibration curves showed good linearity(R^2>0.9908)over a wide concentration range for all compounds.The intra-and interday precision(relative standard deviation)ranged 2.4%–7.0%and 2.6%–8.0%,respectively.The accuracy(relative error)was from-13.0%to 13.2%at all quality control levels.The recovery ranged from 81.1%to 92.5%.The validated method was successfully applied to pharmacokinetic study in rats after oral administration of Qing Gan-Shu Yu-Fang.The results show that one can draw a conclusion that these six active ingredients can be quickly absorbed and play a pharmacodynamic role rapidly in vivo. 展开更多
关键词 PHARMACOKINETICS traditional Chinese medicine prescriptions ultra-performance liquid chromatography with tandem mass spectrometry
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An Automatic Solid Phase Extraction and Ultra-Performance Liquid Chromatography Tandem Mass Spectrometry for Determination of Seven Microcystins at Ultra-Trace Levels in Surface Water
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作者 SHEN Fei XU Yanjuan +1 位作者 WANG Ye CHEN Jing 《Wuhan University Journal of Natural Sciences》 CAS CSCD 2019年第1期30-36,共7页
A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatogr... A method was developed for the detection of seven microcystins(microcystin-LR, RR, YR, LA, LY, LW and LF) in surface water using automatic solid-phase extraction(A-SPE) coupled with ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS). The automated solid-phase extraction system was used to extract microcystins(MCs) from water samples. UPLC-MS/MS was used to determine MCs concentrations in just 5 min. Method detection limits were from 0.3 to 0.9 ng/L, microcystin recoveries ranged from 83.8% to 114%, and the relative standard deviation(RSD) varied from 5.6% to 12.5%. This analytical approach was found to be simple, highly sensitive, accurate, which required little manual operation. Additionally, to validate this analytical method, A-SPE+UPLC-MS/MS was applied to characterize the concentration of MCs in Taihu Lake, Wuxi, China. 展开更多
关键词 MICROCYSTINS AUTOMATIC SOLID-PHASE extraction ultra-performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS)
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Investigations on the degradation of aspartame using high-performance liquid chromatography/tandem mass spectrometry
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作者 Jie-Ping Sun Qiang Han +1 位作者 Xiao-Qiong Zhang Ming-Yu Ding 《Chinese Chemical Letters》 SCIE CAS CSCD 2014年第9期1259-1264,共6页
Aspartame is a widely used sweetener, the long-term safety of which has been controversial ever since it was accepted for human consumption. It is unstable and can produce some harmful degradation products under certa... Aspartame is a widely used sweetener, the long-term safety of which has been controversial ever since it was accepted for human consumption. It is unstable and can produce some harmful degradation products under certain storage conditions. A high-performance liquid chromatography/tandem mass spectrometry method was developed for the simultaneous analysis of aspartame and its four degradation products, including aspartic acid, phenylalanine, aspartyl-phenylalanine and 5-benzyl-3,6- dioxo-2-piperazieacetic acid in water and in diet soft drinks. Aspartame and its four degradation products were quantified by a matrix matched external standard calibration curve with excellent correlation coefficients. The limits of detection were 0.16-5.8 μg/L, which exhibited higher sensitivity than common methods. This method was rapid, sensitive, specific and capable of eliminating matrix interferences. It was also applied to the study of the degradation of aspartame at various pH and temperatures. The results indicated that aspartame was partly degraded under strong acidic or basic conditions and the extent of degradation increased with increasing temperature. 展开更多
关键词 high-performance liquid chromatography/tandem mass spectrometry ASPARTAME Degradation productsCola
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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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阿莫西林胶囊在中国健康人体内的生物等效性研究 被引量:1
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作者 卢俊丽 刘婉莹 +7 位作者 李灿霞 黄丽凤 张婵娟 李艳波 雷雨燕 陈露露 欧阳冬生 颜羽 《广西医科大学学报》 CAS 2024年第1期98-103,共6页
目的:研究阿莫西林胶囊在中国健康人体内的生物等效性。方法:以单中心、开放式、随机、双制剂、两周期、两序列交叉试验设计,共48例受试者(空腹试验和餐后试验各24例),口服0.25 g阿莫西林胶囊受试制剂或参比制剂。高效液相色谱—串联质... 目的:研究阿莫西林胶囊在中国健康人体内的生物等效性。方法:以单中心、开放式、随机、双制剂、两周期、两序列交叉试验设计,共48例受试者(空腹试验和餐后试验各24例),口服0.25 g阿莫西林胶囊受试制剂或参比制剂。高效液相色谱—串联质谱(LC-MS/MS)分析方法测定给药后不同时间阿莫西林的血药浓度,并计算主要药代动力学参数,判定两制剂是否等效。结果:空腹试验显示,受试制剂和参比制剂阿莫西林的药物峰浓度(C_(max))分别为(5483.296±1321.102)ng/mL、(5611.291±1659.407)ng/mL,从时间0到t之间血药浓度—时间曲线下面积(AUC_(0-t))分别为(13255.3±1715.7)h·ng/mL、(13115.5±2091.7)h·ng/mL,从0时到无限时间(∞)的血药浓度—时间曲线下面积(AUC_(0-∞))分别为(13329.4±1718.8)h·ng/mL、(13192.7±2107.1)h·ng/mL,达峰时间(T_(max))均为1.38 h。餐后试验显示,受试制剂和参比制剂阿莫西林的C_(max)分别为(4218.072±780.598)ng/mL、(4156.713±877.752)ng/mL,AUC_(0-t)分别为(13073.9±1584.3)h·ng/mL、(12817.8±1575.5)h·ng/mL,AUC_(0-∞)分别为(13166.8±1606.0)h·ng/mL、(12914.8±1587.2)h·ng/mL,T_(max)均为3.00 h。两种试验制剂C_(max)、AUC_(0-t)、AUC_(0-∞)几何均值比值的90%置信区间(CI)均在可接受的生物等效性范围内(80%~125%)。结论:两种阿莫西林胶囊在中国健康志愿者体内吸收速度和吸收程度生物等效。 展开更多
关键词 阿莫西林 生物等效性 药代动力学 高效液相色谱—串联质谱
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超高效液相色谱-串联质谱法测定水体和底泥中的阿维菌素和伊维菌素
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作者 万译文 杨霄 +4 位作者 谢仲桂 索纹纹 陈湘艺 肖维 李小玲 《湖南师范大学自然科学学报》 CAS 北大核心 2024年第2期136-142,共7页
为建立超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定水产养殖环境(水体及底泥)中阿维菌素和伊维菌素的检测方法。先采用HLB固相萃取柱富集和净化水样,采用PSA和C18吸附剂净化底泥样品;样品中的目标物采用Phenomenex Kinetex C18色... 为建立超高效液相色谱-串联质谱法(UHPLC-MS/MS)同时测定水产养殖环境(水体及底泥)中阿维菌素和伊维菌素的检测方法。先采用HLB固相萃取柱富集和净化水样,采用PSA和C18吸附剂净化底泥样品;样品中的目标物采用Phenomenex Kinetex C18色谱柱分离,以5 mmol/L乙酸铵水溶液和乙腈作为流动相进行梯度洗脱,在电喷雾离子源(ESI)、正离子扫描和多反应监测(MRM)模式下进行测定,外标法定量。在最优实验条件下,阿维菌素和伊维菌素在7.5 min内完成色谱分离分析,目标物在1~100μg·L^(-1)范围内线性关系良好,相关系数均大于0.995。空白水样在0.05,0.50,2.5和5.0μg·L^(-1)共4个添加水平下的回收率为71.6%~88.2%,相对标准偏差(RSD,n=6)在1.51%~8.81%,方法检出限(LOD)为0.02μg·L^(-1),方法定量限(LOQ)为0.05μg·L^(-1);空白底泥在1.0,10.0,50.0和100.0 ng·g^(-1)共4个添加水平下的回收率为75.3%~96.4%,RSD值(n=6)为3.45%~8.99%,LOD值为0.3 ng·g^(-1),LOQ值为1.0 ng·g^(-1)。该方法灵敏度高,重现性好,操作快速简便,适用于水产养殖环境(水体和底泥)中阿维菌素和伊维菌素的分析检测。 展开更多
关键词 超高效液相色谱-串联质谱 阿维菌素 伊维菌素 底泥 水产养殖环境
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