毛细管区带电泳激光诱导荧光间接检测环腺苷单膦酸和环鸟苷单磷酸

研究了影响毛细管区带电泳激光诱导荧光间接检测环腺苷单磷酸和环鸟苷单磷酸的实验条件。ｃＡＭＰ和ｃＧＭＰ的线性范围分别为３０￣５００ｍｇ／Ｌ和１５￣５００ｍｇ／ｌ,其最低检测限分别为９．０ｍｇ／Ｌ和０．５ｍｇ／Ｌ;     

顺序注射环定量光度法在线测定水中总铁

选用邻菲啰啉作为显色剂,采用顺序注射环定量(SIA)光度法,结合一整套系统的PLC程序,成功建立了测定水中总铁的新方法.实验过程中对各条件进行了优化,在最优条件下,体系的检测范围为0～10 mg/L,线性回归方程为A=0.0995c+0.0421(c:mg/L,n=8),相关系数r为0.999 6,方法检出限为0.02 mg/L,相对标准偏差(RSD)为2.3%(0.50 mg/L,n=11)和1.7%(2.00 mg/L,n=11),实际水样的加标回收率为97.1%～102.0%.     

ACF-SPME检测海洋水体中的多环芳烃

使用新型活性炭纤维(ACF)作为固相微萃取(SPME)技术的萃取纤维,检测了海水中的多环芳烃。得到ACF-SPME萃取多环芳烃的最优条件为:在搅拌条件下,盐浓度10%,pH3,温度60℃水浴中直接萃取40min。并确定16种多环芳烃的RSD(n=5)为1.8%～10%、线性范围为0.1～500μg/L、检出限为0.1～100μg/L。对东海近海海水进行了分析,结果表明海水中PAHs浓度在检测限以下,同时进行加标回收实验,得到16种多环芳烃的回收率在80%～128%。     

非水毛细管电泳法分离3种单磷酸腺苷及其应用研究

采用非水毛细管电泳方法对2’-AMP、3’-AMP和5’-AMP 3种单磷酸腺苷进行分离研究,考察了电泳溶液pH*值、非水介质、缓冲溶液对分离的影响。以含50%乙腈的Tris-H3BO3体系为缓冲溶液,在pH*10.0、压差进样(50 mbar,5 s)、柱温25℃、25 kV恒压下进行分离,在波长260 nm处负极检测,各组分可达到基线分离。在质量浓度为1～100 mg/L范围内,3种单磷酸腺苷的线性关系良好,平均回收率为88%～106%,RSD小于4%。该方法应用于核苷样品的测定,结果满意。     

有机脱模剂中多环芳烃的高效液相色谱测定

建立了有机硅类和金属皂类脱模剂中多环芳烃的高效液相色谱测定方法。方法所用色谱柱为多聚C18(LC-PAH)柱,流动相为乙腈/水,采用梯度淋洗方式,开始时为体积分数40%乙腈,28min后变为82%乙腈,48min后变成100%乙腈,保持8min。方法的线性范围为0.10~200mg/L,线性相关系数为0.9993~1.0000,平均回收率分别为68.55%~101.2%(有机硅类)和75.29%~99.89%(金属皂类),精密度RSD分别为1.6%~8.1%(有机硅类)和1.8%~6.8%(金属皂类),检出限(S/N=3)分别为0.05~0.10mg/L(有机硅类)和0.05~0.20mg/L(金属皂类)。该方法可以满足有机硅类和金属皂类脱模剂中多环芳烃的检测要求。     

全二维气相色谱-飞行时间质谱测定地下水中低环多环芳烃及其衍生物

建立了地下水中低环多环芳烃及其衍生物的全二维气相色谱-飞行时间质谱(GC×GC-TOF MS)检测方法。对比研究了液液萃取(LLE)和固相萃取(SPE)对地下水中低环多环芳烃及其衍生物的提取效率,优选液液萃取为前处理方法。在优化条件下,除1,2,3,4-四氢萘(r=0.987 2)和联苯(r=0.989 9)外,其它目标物在0.1~1 000μg/L范围内具有良好的线性关系,相关系数(r)均大于0.99。地下水的平均加标回收率为63.3%~111%,除喹啉的相对标准偏差(RSD,n=6)为24.9%外,其余目标物的RSD均小于9.5%,方法检出限在1.63~14.7 ng/L之间。该方法用于河北地区6个地下水样中低环多环芳烃及其衍生物的检测,4个样品有检出,最高浓度达353 ng/L。     

高效液相色谱法同时测定诺诺感冒片中扑尔敏、扑热息痛、盐酸伪麻黄碱的含量

 采用反相高效液相色谱法 ,在C18柱上以V(甲醇 )∶V(水 ) =2 5∶75的溶液为流动相 (内含 0 .0 5mol/L磷酸二氢钠 ) ,检测波长为 2 0 5nm ,同时分离测定诺诺感冒片中扑尔敏、扑热息痛、盐酸伪麻黄碱的含量。扑尔敏、扑热息痛和盐酸伪麻黄碱的检出限分别为 1.16mg/L ,0 .15mg/L和 1.82mg/L ,其相应的回收率分别为 98.35 % (n =5 ,RSD =1.6 0 % ) ,10 1.16 % (n =5 ,RSD =1.5 0 % )和 98.5 0 % (n =5 ,RSD =1.5 9% )。方法简便、快速 ,重现性好 ,适用于诺诺感冒片的质量检验分析。     

分散液-液微萃取-高效液相色谱法测定环境水样中的多环芳烃

建立了简便、快速、有效的分散液-液微萃取-高效液相色谱-荧光检测(DLLME-HPLC-FLD)测定环境水样中15种多环芳烃(PAHs)的方法。重点探讨了萃取剂的种类和用量、分散剂的种类和用量以及萃取时间等对PAHs萃取效率的影响。在优化的条件下,评价了方法的可靠性。15种PAHs在0.01～10 μg/L范围内呈良好的线性关系,相关系数r均不小于0.9913,峰面积的相对标准偏差(RSD)在2.3%～4.7%之间(n=6)。在优化条件下,富集因子和萃取回收率良好,分别为674～1032和67.4%～103.2%,15种PAHs的检出限(S/N=3)在0.0003～0.002 μg/L之间。建立的方法应用于敖江水样中PAHs的检测,平均加标回收率在79.5%～92.3%之间,RSD在4.3%～6.7%范围内(n=5)。该方法适用于环境水样中痕量PAHs的分析。     

气相色谱-质谱法测定电子电气衬料中多环芳烃和多氯联苯

建立了采用自动索氏萃取-气相色谱-质谱联用检测电子电气产品中多环芳烃和多氯联苯的方法.通过以V(丙酮)∶V(正己烷)＝1∶1为溶剂,一次自动索氏提取材料中多环芳烃和多氯联苯,分别采用H2SO4预处理,再用硅胶柱净化,气相色谱-质谱联用仪检测,该方法对多环芳烃检测限为0.2 mg/kg、多氯联苯检测限为0.1 mg/kg,加标回收率在60%～99%之间,相对标准偏差(RSD)均小于5%,多环芳烃的线性范围在0.1～100 mg/L,多氯联苯的线性范围在0.4～250 mg/L,相关系数(r)均大于0.999.实验结果表明方法能满足电子电气产品材料中多环芳烃和多氯联苯的检测要求.     

超高效液相色谱串联质谱法测定茶叶、茶汤和土壤中氟环唑、茚虫威和苯醚甲环唑残留

建立了绿茶、红茶、普洱茶、茶鲜叶、红茶汤和土壤中氟环唑、茚虫威、苯醚甲环唑残留分析方法。采用Florisil与GCB混合柱净化茶叶和土壤,BondElut C18固相萃取柱富集净化茶汤,超高效液相色谱串联质谱法测定,并对3种农药的质谱裂解和基质效应进行了研究探讨。在0.005～4.0 mg/L浓度范围内均满足线性关系,r>0.9997,仪器检出限LOD<0.002 mg/L;在高、中、低3个添加浓度水平下,不同基质样品(绿茶、红茶、普洱茶、红茶汤、茶鲜叶和土壤)中平均回收率为66.3%～111.5%;相对标准偏差为0.85%～17.6%(n=6);方法定量限LOQ分别为0.005 mg/kg(成茶)、0.002 mg/kg(茶鲜叶、土壤)和0.10!g/L(茶汤)。采用此方法检测40份红茶、绿茶出口样品,1份检出茚虫威残留量为0.014 mg/kg;4份检出苯醚甲环唑残留量为0.012～0.040mg/kg,均未检出氟环唑残留。采用此方法进行茚虫威在茶鲜叶-绿茶加工过程中的消解率、茶叶-茶汤冲泡过程中的浸出率研究,表明茚虫威在绿茶加工过程中的平均消解率为24.8%,3次冲泡的总浸出率平均值为5.2%。     

鲁米诺-铁氰化钾流动注射化学发光法测定头孢拉定

在碱性介质中,铁氰化钾氧化鲁米诺产生化学发光,头孢拉定对该体系有显著的增强作用。基于此并结合流动注射技术建立了测定头孢拉定含量的化学发光新方法。该法线性范围为0.16~160 mg/L,检出限为0.028 mg/L;对80 mg/L的头孢拉定进行平行测定11次,其相对标准偏差为0.99%。用本法对胶囊中头孢拉定进行测定,并初步探讨了该化学发光的反应机理。     

液相色谱-质谱联用分析土壤中的双(2-羟乙基)亚砜

建立了液相色谱 质谱联用技术测定土壤中双(2 羟乙基)亚砜的方法。对影响检测灵敏度的流动相组成、流速、探头温度等因素进行了优化,在优化实验条件下,方法线性范围在0.05～20mg L之间,最低检测质量浓度为0.025mg L(S N>3),对比了3种萃取剂对4种土壤中的双(2 羟乙基)亚砜的萃取率,结果表明,用水作萃取剂的萃取效果最佳,回收率在92%以上,RSD均小于4%。     

Mass spectrometric identification of Rab23 phosphorylation as a response to challenge by cytidine 3',5'-cyclic monophosphate in mouse brain

While the functions and mechanisms of action of adenosine 3',5'-cyclic monophosphate (cAMP) and guanosine 3',5'-cyclic monophosphate (cGMP) are well established and are the basis of the action of a large number of successful pharmaceuticals, the role of a third naturally occurring cyclic nucleotide, cytidine 3',5'-cyclic monophosphate (cCMP), remains to be elucidated. Immobilized metal affinity chromatography (IMAC) was used to selectively extract proteins phosphorylated in mouse brain in response to challenge by cAMP, cGMP and cCMP, followed by matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-ToFMS) and liquid chromatography/electrospray ionization tandem mass spectrometry (LC/ESI-MS/MS) of tryptic digests to identify Rab23 as the first protein reported to be phosphorylated only in response to cCMP.     

固相萃取–高效液相色谱法测定豆芽中4-氯苯氧乙酸钠和6-苄基腺嘌呤的残留量

建立了测定豆芽中4-氯苯氧乙酸钠和6-苄基腺嘌呤的固相萃取–高效液相色谱法。样品以0.1 mol/L的盐酸溶液为提取剂,经C18固相萃取柱净化处理,以乙腈–10 mmol/L乙酸铵水溶液(体积比25∶75)为流动相,Tech Mate C_(18)–ST色谱柱分离,4-氯苯氧乙酸钠和6-苄基腺嘌呤的紫外检测波长分别为228 nm和267 nm,色谱峰面积外标法定量。在0.50~100.00 mg/L浓度范围内,4-氯苯氧乙酸钠的相关系数为0.999 8,精密度在1.3%~8.2%之间(n=6),回收率在103.1%~109.0%之间;在0.05~10 mg/L浓度范围内,6-苄基腺嘌呤相关系数为0.999 9,精密度在0.9%~3.8%之间(n=6),回收率在88.0%~95.4%之间。4-氯苯氧乙酸钠和6-苄基腺嘌呤的检出限(S/N=3)分别为0.24,0.02 mg/kg。该法可以同时完成豆芽中4-氯苯氧乙酸钠和6-苄基腺嘌呤的分析检测。     

Simultaneous determination of Fe(II) and Fe(III) in waters by capillary isotachophoresis

An ITP method for the simultaneous determination of Fe(II) and Fe(III) in waters, based on separation of their EDTA and fluoride complexes, respectively, was developed. The leading electrolyte used consists of chlorides, La(III) as co-counter ion and is buffered with beta-alanine to pH = 3.5. The terminating electrolyte contains caproic acid and L-histidine (pH = 4.5). The method was validated and tested with samples of artificial, ground and treated water with good results, comparable to those obtained by other analytical techniques. Fe(II) and Fe(III) up to 20 mg/L were measured with an RSD = 1.4-1.5% and detection and determination limits of 0.8-0.9 and 3.0-3.5 mg/L, respectively. The ITP method can be recommended for routine utilization in hydroanalytical laboratories.     

薄层扫描快速检测发酵液中琥珀酸

基于CuSO4与发酵液中琥珀酸的显色反应,在硅胶板上不经层析展开使用薄层扫描定量分析琥珀酸含量.在0～12 g/L范围内,测定波长680 nm,参比波长500 nm条件下,琥珀酸浓度与显色斑吸光度呈良好线性关系.方法检出限(3 S/k)为0.028 mg/L,回收率94.80％～96.12％,相对标准偏差≤3.5％(n...     

高效液相色谱法测定我国北方红枣中环磷酸腺苷的含量

采用高效液相色谱（HPLC）法准确测定环磷酸腺苷（cAMP）含量,并对我国北方红枣中的cAMP含量进行测定.以Hibar ODS-C18（250 mm×4.6 mm,5 μm）为色谱柱,流动相为甲醇:2%醋酸（体积比为5:95）,流速0.5 mL/min,检测器为Waters 996,检测温度为25℃,检测波长为254 nm.标准曲线在0.1~1.0 mg/mL范围内线性良好,加标回收率为102.1%,相对标准误差为0.63%.同时,采用的条件能将红枣中cAMP与其他成分的峰完全分离,发现不同产地的红枣中cAMP含量不同,新疆地区所产红枣的质量分数最高,能达到372 μg/g.方法可准确测定我国北方红枣中环磷酸腺苷的含量,灵敏度高,可为红枣中cAMP的提取和高值化利用提供重要的技术依据.     

Determination of trace metals by capillary electrophoresis

A new analytical procedure is developed using a strong complexing agent, 1,10-phenanthroline (Phen), for direct UV detection of Zn, Mn, Cu, Co, Cd, and Fe at microg/L concentrations in environmental water samples. The metal chelates formed showed different electrophoretic mobilities and solved the comigration problem for capillary electrophoresis (CE) separation of free metal ions. To obtain stable metal-Phen chelates during the capillary zone electrophoresis (CZE) run, both pre-column and on-column complexation are required and threefold excess of Phen over metal ions should be added to the sample. The optimized background electrolyte (BGE) consists of 30 mM hydroxylamine hydrochloride and 0.1% methanol at pH 3.6. Under hydrodynamic sampling, CE run at + 20 kV in 65 cm x 0.05 mm ID fused-silica column with detection at 265 nm, baseline separation, satisfactory working ranges (10 microg/L to 5.5 mg/L), sensitive detection limits (1-3 microg/L), good repeatability for migration times (relative standard deviation, RSD 0.36-0.81%, n = 5), peak area (RSD 3.2-4.2%, n = 5) and peak height (RSD 3.2-4.5%, n = 5) were obtained for the metal cations investigated. The reliability of the method was established by parallel determination using the inductively coupled plasma-atomic emission spectrometry (ICP-AES) method giving results within statistical variation. The procedure developed is shown to provide a quick, sensitive, precise, and economic method for simultaneous determination of metal cations that can form stable chelates with Phen.     

A flow injection chemiluminescence system for the determination of isoniazid

A chemiluminescence (CL) flow system is described for the determination of isoniazid based on its enhancement on the chemiluminescence (CL) emission produced upon mixing a hexacyanoferrate(III) solution with an alkaline luminol solution. The system responds linearly to isoniazid concentration in the range 0-1 mg/L with a detection limit (3sigma) of 0.03 microg/L, relative standard deviation (RSD) of 1.2% for 0.1 mg/L isoniazid (n = 11). The system has been successfully applied to the determination of isoniazid in pharmaceutical preparations.