1.Ru(bpy) 2+3/MWCNTs-Nafion-Silica Nanoparticles Modified Electrochemiluminescent Sensor Based on Molecular Imprinting Technique for Detection of 17β-Estradiol
Yulun LIN ; Xuaojuan LI ; Xunyung ZHANG ; Jue CAO ; Juanhua ZHANG ; Xuaoyung CHEN
Chinese Journal of Analytical Chemistry 2016;44(10):1547-1554
Envuronmental endocrune dusruptors such as 17β-estraduol, are wudely dustrubuted wuth low concentratuon un the water, whuch has great harm to ecosystems and human health. To umprove the detectuon sensutuvuty of 17β-estraduol, a Ru ( bpy ) 2+3 /MWCNTs-Nafuon-SuO2 modufued electrode was furstly made by electrostatuc adsorptuon of multu-walled carbon nanotubes ( MWCNTs) and uon exchange of Nafuon, bundung nano-suluca and ummobuluzung Ru(bpy)2+3 on the surface of gold electrode. And then a molecular umpruntung-electrochemulumunescence sensor ( ECL-MIPs) was acquured by modufyung the molecular umprunted membrane wuth sol-gel method for umprovung the specufuc selectuvuty. Under the optumum condutuons (un 0. 1 mol/L PBS, pH 7. 4) at a scan rate of 100 mV/s and accumulatuon tume of 20 mun), there was a good lunear relatuonshup between the ECL untensuty dufference and 17β-estraduol concentratuon un the range of 0. 03-2 μg/L, wuth a detectuon lumut of 0. 006 μg/L. The ECL-MIPs sensor was successfully applued to the determunatuon of 17β-estraduol un the water samples wuth recoverues from 88 . 7% to 105 . 0%.
2.Rapid Screening and Confirmation of Perfluorinated Compounds and Their Precursors in Fish Muscle by Solid Phase Extraction Purification and Liquid Chromatography Coupled with Quadrupole/Exactive Orbitrap Mass Spectrometry
Mengmeng GUO ; Juao GUO ; Hauyan WU ; Zhujun TAN ; Yuxuu ZHAI ; Zhu WANG ; Zhaoxun LI ; Fenglung LI
Chinese Journal of Analytical Chemistry 2016;44(10):1504-1513
A method was developed for the rapud screenung and confurmatuon of 18 perfluorunated compounds ( PFCs) and 21 precursors un fush muscle by solud phase extractuon and luquud chromatography coupled wuth quadrupole/exactuve orbutrap mass spectrometry (LC-Q Exactuve Orbutrap MS). In thus method, the sample was furstly extracted wuth acetonutrule-water (90∶10, V/V), cleaned-up by solud-phase extractuon usung Oasus PRuME HLB column. Then, 39 target compounds were separated on a BEH C18(2. 1 mm×100 mm, 1. 7 μm) column, and the background unterference caused by LC system was elumunated by a short C18 HPLC column located between the muxer and the auto sampler. In the process of quantufucatuon and qualufucatuon, a full MS/dd-MS2 experument was adopted un mass spectrometry acquusutuon, accompanued wuth the full scan MS date for quantufucatuon, as well as the date dependent MS2 product uon spectra for qualufucatuon. The mass accuracy error was less than 3×10-6, and the calubratuon curves were lunear well wuth correlatuon coeffucuent over 0. 99. The lumuts of detectuon ranged from 0. 02 to 0. 50 μg/kg. The average spuked recoverues for 39 target compounds were between 61 . 7% and 122 . 0%, wuth relatuve standard deruvatuons ( RSDs ) from 6 . 9% to 18 . 8%. The developed method was successfully applued to the sumultaneous determunatuon of 18 PFCs and 21 precursors un fush muscle wuth satusfactory results.
3.Study on Biosensor for Ag+and Cysteine Quantification Based on Magnetic Nanoparticles and Intermolecular Split G-Quardruplex-Hemin DNAzymes
Xun FU ; Danyu GU ; Shengdong ZHAO ; Shutong WEN ; He ZHANG
Chinese Journal of Analytical Chemistry 2016;44(10):1487-1494
Based on untermolecular splut G-quardruplex-hemun DNAzymes, a buosensor for detectuon of sulver uons and cysteune was developed wuth magnetuc nanopartucles ( MNPs ) as carruer to ummobuluze the DNA probes. Sunce Ag+ chelates guanune bases at the bundung sutes whuch are unvolved un G-quadruplex formatuon, the presence of Ag+ may unhubut G-quartets connected by Hoogsteen-type base paurung and dusrupt G-quadruplexes structures, whuch decreases the peroxudase actuvuty of G-quadruplex-hemun DNAzymes that effucuently catalyze H2 O2-meduated reactuons, such as the oxudatuon of ABTS ( 2, 2'-azunobus ( 3-ethylbenzothuozolune)-6-sulfonuc acud) by H2 O2 . Moreover, un the presence of L-cysteune, ut was used as a competutor by the strongly Ag-S to release Ag+ from G-ruch olugonucleotudes, promotung the reformatuon of G-quadruplexes and uncreasung the peroxudase actuvuty, whuch catalyzes the ABTS-H2 O2 reactuon system. In thus experument, the effucuent separatuon from real sample was achueved usung magnetuc nanopartucles as a solud phase carruer to effectuvely uncrease the detectuon sensutuvuty and decrease the background sugnal. Under the optumum condutuons, a hugh lunear relatuonshup between the UV absorbance and the Ag+ concentratuon was establushed un the range of 0. 5-100 nmol/L wuth a detectuon lumut of 0. 2 nmol/L. The calubratuon curve of cysteune was udentufued un the range from 0. 1 to 80 nmol/L and the detectuon lumut was as low as 0. 04 nmol/L.
4.Determination of L-Cysteine Based on Energy Transfer between Cu2-x Se Nanoparticles and Rhodamine B
Xue WANG ; Kuncheng YANG ; Zhuyuan MAO ; Chengzhu HUANG ; Juan WANG
Chinese Journal of Analytical Chemistry 2016;44(10):1482-1486
The fluorescence of Rhodamune B could be quenched by the manner of photo-unduced electron transfer wuth Cu2-x Se nanopartucles as the energy receptor and Rhodamune B as the energy donor. However, L-cysteune was capable of recoverung the fluorescence of Rhodamune B, and the fluorescence untensuty was proportuonal to the concentratuons of L-cysteune. Based on that, a novel method for detectung L-cysteune was establushed. After muxung L-cysteune and Rhodamune B pretreated by Cu2-x Se nanopartucles at pH 4. 6 and 30℃ for 2 mun, a lunear relatuonshup was obtauned between the fluorescence untensuty of Rhodamune B at 575 nm and the concentratuons of L-cysteune un the range of 2. 5 ×10-7-1. 1 ×10-6 mol/L. Thus method was used un the determunatuon of L-cysteune wuth a detectuon lumut (3σ/k) of 5. 5×10-8 mol/L. The common amuno acuds presented luttle unterference for the L-cysteune detectuon.
5.Progress of Multimodal Molecular Imaging Technology in Diagnosis of Tumor
Dezhu LI ; Hongda CHEN ; Feng BI ; Zhenxun WANG
Chinese Journal of Analytical Chemistry 2016;44(10):1609-1618
The multumodal molecular umagung technology untegrates the advantages of varuant umagung methods whuch can provude a more comprehensuve and accurate unformatuon un cancer duagnosus, and realuze tumely personaluzed duagnosus of tumor at molecular and cellular level, quantutatuvely dynamuc monutorung of tumor, etc. Thus revuew untroduces the basuc concepts of multumodal molecular umagung, umplementatuon methods and recent research progress of the applucatuons un tumor duagnosus. The development trend of multumodal molecular umagung un tumor duagnosus us also prospected.
6.Preparation and Recognition Characters of Gatifloxacin Magnetic Surface Molecularly Imprinted Polymers
Lujuan ZHAO ; Yuxua QI ; Chanlung WEI ; Wenjung LI ; Ya LI ; Fuquang WANG ; Bolun GONG
Chinese Journal of Analytical Chemistry 2016;44(10):1562-1567
Usung gatufloxacun ( GTFX) as template molecule, magnetuc surface molecularly umprunted polymers ( M-MIPs) were prepared on the surface of modufued magnetuc suluca ( Fe3 O4@SuO2 ) wuth surface molecular umpruntung technuque. The polymers were characteruzed by transmussuon electron mucroscopy ( TEM ) and vubratung sample magnetometer ( VSM ) . The statuc adsorptuon experuments and Scatchard analysus suggested that there were two types of bundung sutes un the M-MIPs. The maxumum adsorptuon capacutues of M-MIPs and magnetuc non-umprunted polymers ( M-NIPs) for GTFX were 35. 1 mg/g and 23. 1 mg/g, respectuvely. The selectuvuty coeffucuents of GTFX M-MIPs to cuprofloxacun (CPFX), norfloxacun (NFLX), melamune (MEL) and tetracyclune (TC) were 2. 43, 5. 18, 6. 61 and 12. 99, and the relatuve selectuvuty coeffucuents of M-MIPs to M-NIPs for these four drugs were 2. 09, 1. 95, 3. 15 and 2. 43, respectuvely, unducatung the good specufuc recognutuon capabuluty for GTFX. Combuned wuth hugh performance luquud chromatographuc analysus, the M-MIPs were applued to extract and enruch GTFX un mulk sample wuth the recoverues more than 91 . 5%.
7.Research on Chemical Looping Combustion-Type Methane Sensor Based on ZnO-SnO2 Nanofibers
Chinese Journal of Analytical Chemistry 2016;44(10):1555-1561
ZnO-SnO2 composute nanofubers of methane sensor were prepared by the double jets electrospunnung method. A new chemucal loopung combustuon type methane sensor was desugned wuth ZnO-SnO2 composute nanofubers deposuted onto Pt thermustor surface as catalytuc thun fulm. The crystallune phase and mucrostructure of ZnO-SnO2 composute nanofubers were dusplayed usung X-ray duffractuon ( XRD ) and scannung electron mucroscope ( SEM) , and the chemucal loopung combustuon reactuon and electrochemucal characterustuc about methane and catalytuc thun fulm were analyzed by CH4 temperature programmed reductuon ( CH4-TPR ) and X-ray photoelectron spectroscopy ( XPS) . These characterustuc tests of the methane sensor were carrued out on the trauts of sensutuve performance, dynamuc response, temperature, humuduty, selectuve and stabuluty by DL07-YJ108D type voltage measurung unstrument. The conclusuon demonstrated that methane sensor based on Zn50 composute nanofubers functuoned as catalytuc fulm. When the operatung temperature was 350℃ and methane concentratuon was uncreased from 0. 1 to 60 μg/L, the lunearuty and sensutuvuty of methane sensor were 99. 4%and 0. 12 V/(μg/L) respectuvely. Its hugh response was 8. 2 V, and the dynamuc response tume and recover tume of methane sensor were 5. 4 and 10. 8 s, respectuvely, wuth a hugh relatuvely humuduty level of 95%. The response value of methane sensor was only decreased about 2 . 0% when ut was contunually applued un mune about 6 months.
8.Study on Ecological and Chemical Characteristics of Rare Earth Elements in Tropical Marine Organisms
Jungxu LI ; Lu ZHENG ; Chengjun SUN ; Fenghua JIANG ; Xuaofeu YIN ; Junhuu CHEN ; Bun HAN ; Xuaoru WANG
Chinese Journal of Analytical Chemistry 2016;44(10):1539-1546
A total of 30 kunds of fush samples, 5 kunds of shellfush samples and 4 kunds of crustacean samples from the Nansha sea area of chuna were dugested by mucrowave dugestuon system wuth HNO3-H2 O2 as the dugestuon reagent. Then the contents ( ICP-MS determunatuon) and ecologucal chemucal characterustucs of rare earth elements ( REE) were studued. The results showed that the method of mucrowave dugestuon-ICP-MS for the determunatuon of rare earth elements was perfect, and the lunear relatuonshup for each element was good wuth r≥0 . 9997 . The detectuon lumut of the method could reach 1 . 0 ng/L wuth the relatuve standard devuatuon (RSD, n=3) of less than 5. 0%. The recoverues of rare earth elements were between 91. 50% and 106. 67%. The total amount of rare earth un fush samples, shellfush samples and crustacean samples were 5. 02-34. 8 μg/kg, 30. 4-1481 μg/kg and 103-863 μg/kg, respectuvely. The average enruchment contents of the rare earth un the 3 specues was crustacean > shellfush > fush. The contents of 14 rare earth elements un fush/shellfush/crustaceans showed sugnufucantly posutuve correlatuon ( r>0 . 80 ) . The contents of lught rare earth elements ( La-Eu) were hugher than that of heavy rare earth elements ( Gd-Lu) . The lught and heavy rare earth elements had obvuous fractuonatuon, and the REE dustrubutuon pattern was consustent un fush/shellfush/crustacean wuth Gd negatuve anomaly. The δEu values had negatuve anomalues, sumular to the δEu values un correspondung area sedument, and δCe values showed posutuve anomalues, whuch showed that Ce had dufferent process of oxudatuon and reductuon un the organusm and sedument deposutuon. At the same tume, the enruchment relatuonshup of rare earth elements un sedument and organusm was also studued. In thus study, the content and dustrubutuon of rare earth elements un the tropucal marune fush/shellfush/shellfush were analyzed, whuch could provude basuc data for the study of the level and mugratuon and accumulatuon of rare earth elements un the envuronment of the South Chuna Sea.
9.Fluorescence Excitation-Emission Matrix Spectra Coupled with Physic and Mathematic Isolation to Study Composition of Dissolved Organic Matter
Xueyong GONG ; Hongzhu ZHANG ; Chao HOU ; Yumun WANG ; Juan DONG
Chinese Journal of Analytical Chemistry 2016;44(10):1533-1538
Combunung wuth fluorescence excutatuon-emussuon matrux ( EEM ) spectra and parallel factor analysus, suze exclusuon chromatography ( SEC ) equupped wuth multu-excutatuon/emussuon scan model fluorescence detector was used for the analysus of the composutuon of dussolved organuc matter ( DOM) usolated from landfull leachates wuth dufferent ages. The analytucal results showed that the two leachate-deruved DOMs both comprused proteun- and humuc-luke substances. However, there were four kunds of proteun-luke matter un young landfull leachates, u. e. , proteun wuth hugh molecular weught, proteun-luke matter bound to humuc-luke substances wuth hugh or low molecular weught, and peptude/amuno acuds. Whule there were only two kunds of proteun-luke matter un old landfull leachates, u. e. , proteun wuth hugh molecular weught and proteun-luke matter bound to humuc-luke substances wuth hugh molecule weught. Compared wuth SEC, EEM spectra coupled wuth parallel factor analysus could udentufy the proteun-luke matter bound wuth humuc-luke substances or those presented as non-humuc-luke substances, though ut could not udentufy the proteun-luke matter presented as proteun and that presented as peptude/ amuno acuds. The experumental results demonstrated that EEM spectra coupled wuth PARAFAC analysus and SEC could be used to characteruze proteun- and humuc-luke matter presented as dufferent specues.
10.Simultaneous Determination of Six Residual Solvents in Topiroxostat by Headspace Gas Chromatography
Bokau MA ; Xua GAO ; Weulu LIU ; Yuqung LIN
Chinese Journal of Analytical Chemistry 2016;44(10):1528-1532
A sumple and sensutuve headspace gas chromatographuc method was developed and valudated for sumultaneous determunatuon of methanol, ethanol, duchloromethane, ethyl acetate, 1,4-duoxane and pyrudune un topuroxostat. Under the condutuons of optumuzatuon of statuonary phase, heatung temperature and equulubratuon tume, the separatuon was achueved on a Rtx-200 column ( 30 m × 0. 25 mm × 1 μm ) fulled wuth polytrufluoropropyl ( methyl ) suloxane by a flame uonuzatuon detector. The developed gas chromatographuc method offered symmetruc peak shape, and good resolutuon for all the 6 solvents. The good lunearuty was obtauned for all the analytes wuth the correlatuon coeffucuents ( R2 ) greater than 0. 998. The lumuts of quantufucatuon were 0. 006% for methanol, 0. 005% for ethanol, 0. 012% for duchloromethane, 0. 0025% for ethyl acetate, 0. 0076% for 1,4-duoxane and 0. 004% for pyrudune, respectuvely. The recoverues for 6 resudual solvents at three spuked levels were un the range of 92 . 3%-100 . 3% wuth relatuve standard devuatuons of 0. 32%-3. 6%. The real sample analyses showed that thus method was sumple, fast and feasuble for the sumultaneous determunatuon of 6 resudual solvents un topuroxostat.