英语翻译2 .Experimental2 .1.Reagents and chemicalsAll chemicals

英语翻译
2 .Experimental
2 .1.Reagents and chemicals
All chemicals used were of analytical grade unless stated otherwise.Acetic acid,acetonitrile,ascorbic acid,citric acid monohydrate,lead(IV)oxide,di-so-dium hydrogen phosphate dihydrate,were purchased from Merck (Darmstadt,Germany).Ammonium hydroxide 25% (m/v),dichloromethane,methanol (HPLC grade),sodium acetate,sodium perchlorate monohydrate,para-toluenesulfonic acid ( p-TSA) were obtained from J.T.Baker (Phillipsburg,NJ,USA).Brilliant green and N,N,N9,N9-tetramethyl-1,4-phenylenediamine dihydrochloride (TMPD) were from Aldrich (Steinheim,Germany),and celite from Acros (Geel,Belgium).N,N-Dimethylformamide
was bought from Rathburn (Walkerburn,UK).Leuco-malachite green and 1-pentanesulfonic acid
(sodium salt) were delivered by Sigma (St.Louis,MO,USA) and malachite green oxalate (Vetrenal
reference standard) by Riedel-de-Hae¨n (Seelze,Ger-many).Aromatic sulfonic acid-bonded SPE columns (3 ml; 500 mg) were purchased from J.T.Baker.Water was of Milli-Q quality (Millipore,Bedford,USA).
2 .2.Apparatus
Screw-capped polypropylene tubes (50 ml and 6 ml) were supplied by Sarstedt (Numbrecht,Germany).Series of SPE columns equipped with 75-ml reservoir adapters were processed simultaneously using a vacuum manifold (J.T.Baker).Samples were dried using an evaporation manifold from Pierce (Rockford,IL,USA).
2 .5.LC–MS–MS analysis
For LC–MS–MS analysis,10-ml aliquots were injected on an HPLC system consisting of two HPLC pumps (PE200 series,Applied Biosystems),an autowas sampler (PE 200 series,Applied Biosystems) and an API-365 MS detector (Applied Biosystems).The LC–MS–MS was controlled by Analyst software package (version 1.1).The HPLC column was a Phenomenex Luna C (5032 mm,Phenomenex,Torrance,USA) with guard column (SecurityGuard C18 4*2 mm,Phenomenex).The mobile phase was a mixture of 50 mM ammonium acetate,pH 4.4,and acetonitrile (2:3,v/v) flowed at 200 ml /min.Before the eluent was introduced into the ionization chamber for MS detection of the analytes,the effluent was passed through a post-column reactor filled with lead(IV)oxide and celite (see Section 2.4).
The MS was equipped with an ESI interface operating at an ionization voltage of +5500 V and a
source temperature of 400 8C.The entrance,declustering and focusing potentials were set at 29,40 and 180 V,respectively.Tandem MS analysis was performed using the multi-reaction-monitoring (MRM) mode.Collision energy (CE) was optimized for each product-ion trace measured.The following traces were monitored:m/z 329.3→m/z 165.0 (CE 75 V),m/z 329.3→m/z 208.0 (CE 55 V),m/z 329.3→m/z 313.3 (CE 45 V) and for the internal standard m/z 385.0→m/z 341.0 (CE 50 V) (Fig.1).

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2.实验性
2 .1.试剂和化学制品
使用的所有化学制品除非陈术否则是分析成绩.乙酸,乙腈,抗坏血酸,柠檬酸一水化物,主角(IV)氧化物,di-so-dium氢磷酸盐二水合物,从默克(达姆施塔特,德国)被购买了.氢氧化铵25% (m/v),二氯甲烷,甲醇(高性能液体色谱等级),钠醋酸盐,钠高氯酸盐一水化物,巴拉toluenesulfonic酸(p-TSA)从J.T.贝克(Phillipsburg,NJ,美国)得到了.精采绿色和N,N,N9,N9四甲基1,4苯二胺二氢氚化物(TMPD)是从从Acros (Geel,比利时)的Aldrich (Steinheim,德国)和钙铁石.N,N二甲替甲酰胺
从Rathburn (Walkerburn,英国)被买了.Leuco绿沸铜绿色和1-pentanesulfonic酸
(钠盐)交付Sigma (圣路易斯,MO,美国)和绿沸铜绿色乙二酸酯(Vetrenal
参比标准器)由RiedeldeHae¨n (Seelze,德国).芳香磺基的酸保税的SPE专栏(3 ml; 500毫克)从J.T.贝克被购买了.水是Milli-Q质量(微孔,贝得福得,美国).
2 .2.用具
sarstedt供应螺丝加盖的聚丙烯管(50 ml和6 ml) (Numbrecht,德国).使用真空歧管(J.T.贝克),SPE专栏系列装备75ml水库适配器同时被处理了.样品被烘干了使用从皮尔斯(罗克福德,IL,美国)的蒸发多头管.
2 .5.LC-MS-MS分析
对于LC-MS-MS分析,10ml整除数在包括二个高性能液体色谱泵浦(PE200系列,应用的生物系统),autowas取样器(PE 200系列,应用的生物系统)和API-365 MS探测器(应用的生物系统)的高性能液体色谱系统被注射了.LC-MS-MS是由Analyst软件包(版本控制的1.1).高性能液体色谱专栏是Phenomenex有保护柱的(SecurityGuard C18 4*2 mm,Phenomenex)月神C (5032 mm,Phenomenex,Torrance,美国).流动相是50 mM混合物乙酸胺、酸碱度4.4和乙腈(2 ：3,v/v)流动在200 ml /min.在洗提液被介绍了入分析物的MS侦查的之前电离室,流出物通过了岗位专栏反应器充满主角(IV)氧化物和钙铁石(参见第2.4部分).
MS用在+5500 V和a电离电压的一ESI接口操作装备了
来源温度400 8C.入口,declustering的和聚焦的潜力被设置了在29,40和180 V,分别.使用多反应监视(MRM)方式,纵排MS分析执行了.碰撞能量(铈)为被测量的每生产踪影被优选了.以下踪影被监测了：m/z 329.3→m/z 165.0 (铈75 V),m/z 329.3→m/z 208.0 (铈55 V),m/z 329.3→m/z 313.3 (铈45 V)和内部标准的m/z 385.0→m/z 341.0 (铈50 V) (图1).
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