高效液相色谱法测定除草剂中二氯喹啉酸的含量

本文报道酸抑制反相色谱法测定除草剂中二氯喹啉酸的含量，该法采用ＰＣ８－１０／Ｓ２５０４（４．０ｍｍｉ．ｄ．×２５０ｍｍ，１０μｍ）柱，以甲醇－０．１％醋酸为流动相，紫外检测波长为２４０ｎｍ，０．０８ＡＵＦＳ，以２，４－二硝基氯苯为内标物，样品用四氢呋喃提取，该法灵敏度及回收率高，结果定量准确，操作简便可靠。     

高效液相色谱法和因子分析—紫外光度法测定荧光增白剂中两种成分

本文采用两种同时测定荧光增白剂工业产品中，１，４－（２，４′－氰基苯乙烯基）苯（记为ＥＢ）和异构体１，４－双（２－氰基苯乙烯基）苯（记为ＥＲ）两组分的方法，一种是ＨＰＬＣ法，采用Ｓｈｉｍ－ｐａｃｋＣＬＣ－ＳＩＬ柱（５μｍ，６．０ｍｍｉ．ｄ×１５０ｍｍ）正己烷－乙酸乙酯（９０：１０Ｖ／Ｖ）为流动相，流速２ｍＬ／ｍｉｎ，柱温３０℃检测波长ＵＶ３６０ｎｍ方法简单，准确，快速，另一种是因子分析－紫外光度法     

反相高效液相色谱法测定牙膏中的甘草次酸

采用反相高效液相色谱法测定了牙膏中的甘草次酸。在ＹＷＧ Ｃ１８（４０ｍｍｉ．ｄ．×２５０ｍｍ,１０μｍ）色谱柱上,以Ｖ（甲醇）∶Ｖ（００１ｍｏｌ／ＬＫＨ２ＰＯ４）＝８５∶１５（ｐＨ３０）的溶液为流动相,流速为１０ｍＬ／ｍｉｎ,紫外检测波长为２５４ｎｍ,室温下检测。甘草次酸用甲醇提取。甘草次酸的平均回收率为９９６１％～１０１６７％,样品测试相对标准偏差为１８５％～３１６％。方法操作简便、快速和准确。     

柱后衍生高效液相色谱法测定鸡肉中莫能菌素残留量

样品用甲醇－水溶液匀浆、提取后过滤,再用二氯甲烷进行液－液萃取,然后通过Ｓｅｐ－Ｐａｋ柱进一步净化。净化后的样液与香兰素衍生试剂在酸性和加热条件下进行柱后衍生,反应产物在５２０ｎｍ波长处测定。衍生剂：香兰素３０．０ｇ＋浓硫酸２０ｍＬ＋甲醇９５０ｍＬ,流速：０．７ｍＬ／ｍｉｎ;色谱柱：μ－ＢｏｎｄａｐａｋＴＭＣ１８３．９ｍｍｉ．ｄ．×３００ｍｍ,或相当的色谱柱;流动相：Ｖ（甲醇）Ｖ（水）Ｖ（磷酸）＝９４０６０１,流速０．７ｍＬ／ｍｉｎ;柱后反应室：体积大于１．４ｍＬ的不锈钢管（３００ｃｍ×１ｍｍｉ．ｄ．）。     

聚乙类吡咯烷酮动态涂敷毛细管电泳柱分离碱性蛋白质

以聚乙烯吡咯烷酮（ＰＶＰ）为添加剂对毛细管柱进行动态修饰,用于碱性蛋白分离。对４种碱性蛋白质进行分离,实验结果表明聚乙烯吡咯烷酮能够很了地抑制电不渗流（ＥＯＦ）及碱性蛋白在石英毛细管壁上的吸附作用。在ｐＨ４．０,ＰＶＰ浓度（Ｗ／Ｖ）为０．４％时,ＥＯＦ仅为１．３５×１０＾－９ｍ＾２／Ｖ．ｓ,平均柱效可达５×１０＾５理论塔板数／ｍ。每次运行之间（ｎ＝６）,天与天之间（ｎ＝６）,迁移时间的相对标准偏差     

反相高效液相色谱法测定杀虫剂中吡虫啉的含量

报道了反相色谱法测定杀虫剂中吡虫啉的含量，该法采用ＹＷＧ－Ｃ１８（２５０ｍｍ×４．０ｍｍ，１０μｍ），柱，以甲醇－水（含０．１％二乙胺，ｐＨ５．０），（３５：６５，Ｖ／Ｖ，１．０ｍＬ／ｍｉｎ）为流动相，紫外检测波长为２７０ｎｍ，０．１６ＡＵＦＳ，样品可直接用甲醇超声提取。样品中吡虫啉平均回收率≥９７．４３％，相对标准偏差≤２．１％。     

氯菊酯胺菊酯混合防蛀剂的气相色谱法测定

用３％ＯＶ－１０１２ｍ×３ｍｍｉ．ｄ．玻璃或不锈钢柱,以邻苯二甲酸二（２－乙基）己酯为内标,在柱温２２３℃时同时测定氯菊酯胺菊酯混合防蛀剂中有效成分——氯菊酯和胺菊酯的质量分数。方法中氯菊酯和胺菊酯的平均变异系数分别为０．２０％和０．１９％。     

以乙基紫为活性物质的聚氯乙烯膜氰化亚金电极的研制和应用

以碱性染料为活性物质制备２０余种不同组分ＰＶＣ膜Ａｕ（ＣＮ）２＾－电极，确定较佳膜组成为乙基紫０．９９％，邻苯二甲酸二丁酯６９．２％，ＰＶＣ粉２９．８％。该电极对Ａｕ（ＣＮ）２＾－浓度在５．０×１０＾－７￣１．０×１０＾－２ｍｏｌ／Ｌ范围内接近能斯特响应；斜率为５５．７ｍＶ（３０℃）。稳定性与选择性较好。该电极制备简单，使用方便，已成功用于氰化镀金液中金的测定。     

气相色谱法分离和测定对甲硫基苯酚

采用气相色谱法分离和测定对甲硫苯酚。在Ф６ ×１ ．５ ×１ ５００ ｍ ｍ 玻璃柱内填充５ ％ Ｏ Ｖ１０１／ Ｃｈｒｏｍ ｏｓｏｒｂ Ｗ Ａ Ｗ Ｄ Ｍ Ｃ Ｓ 的色谱柱上,对甲硫基苯酚与内标物磷酸三丁酯及杂质之间具有较好的分离效果;而且以磷酸三丁酯为内标物时其重量校正因子相当稳定,即 ｆｗ ． Ａ ＝ ０ ．９４８ ±０ ．００５ ４（ｎ ＝ ９ ,α＝ ０ ．０５） 。该方法操作简便、快速、准确。对同一试样的８ 次平行独立测定其标准偏差为０ ．２５ ,变异系数为０ ．００７ ２ 。并且,该方法的３ 次加入法回收率达９８ ．１８ ％ ～９９ ．２２ ％ 。     

反相高效液相色谱法同时测定果汁中8种添加剂

建立了反相高效液相色谱法（ＲＰ－ＨＰＬＣ）同时直接测定进口果汁中柠檬黄和苋菜红等８种添加剂含量的方法。色谱柱为Ｈｙｐｅｒｓｉｌ　ＢＤＳ　Ｃ１８柱（２５０ｍｍ×４．０ｍｍｉ．ｄ,５μｍ）,流动相为甲醇／０．０１ｍｏｌ／Ｌ乙酸铵,梯度洗脱,流速为 １．０ ｍＬ／ｍｉｎ,柱温为 ４０℃,ＤＡＤ紫外检测器波长为 ２３０ ｎｍ。在此色谱条件下,各组分在１０ ｍｉｎ内均得到良好分离。平均回收率为 ９０％～１１４％,相对标准偏差 １．３％～８．０％。     

固相萃取富集高效液相色谱法测定苯氧乙酸和2,4-二氯苯氧乙酸

建立了以固相萃取技术进行富集 ,高效液相色谱法进行分离和检测苯氧乙酸和 2 ,4 二氯苯氧乙酸的方法。环境水中的苯氧乙酸和 2 ,4 二氯苯氧乙酸用Sep PakC18Cartridge进行固相萃取。液相色谱的条件是 :Shim PackCLCODS柱为分析柱 ;甲醇 水 (9∶1,V/V)为流动相 ;流速为 1mL/min ;在UV 2 75nm波长下进行检测。本法具有良好的灵敏度和重现性     

Determination of trichloroacetate in human serum and urine by ion chromatography

A simple and rapid ion chromatographic method has been developed for the determination of trichloroacetate in human serum and urine. Two short (50 x 5 mm i.d.) low-capacity anion-exchange resin columns in series were used as the analytical column and a mixture of 35 mM sodium hydroxide, 20 mM p-hydroxybenzonitrile and 2% V/V acetonitrile (pH 12.3) as the eluent. The calibration graph was rectilinear from 0.3 to 33 mg l-1 of trichloroacetate at 10 microS with a detection limit (3 sigma) of 0.08 mg l-1. The recovery of trichloroacetate, obtained by analysing spiked serum and urine samples, was in the range 98.2-101% and the coefficient of variation was always less than 3.0%.     

离子色谱法测定奶制品及蜂王浆中的乙酰胆碱

建立了奶制品及蜂王浆中乙酰胆碱的离子交换/电导检测离子色谱分析方法.样品经去离子水超声提取,离子交换/电导检测离子色谱法测定,外标法定量.采用IonPac CS17(250 mm x4.0 mm i.d.)分析柱,流动相为甲基磺酸,梯度洗脱,流速1.0 mL/min,柱温30℃,检测池温度35℃.实验结果表明,氯化乙酰...     

Ultra high-performance liquid chromatography of porphyrins in clinical materials: column and mobile phase selection and optimisation

Ultra high-performance liquid chromatographic (UHPLC) systems on columns packed with materials ranging from 1.9 to 2.7 μm average particle size were assessed for the fast and sensitive analysis of porphyrins in clinical materials. The fastest separation was achieved on an Agilent Poroshell C(18) column (2.7 μm particle size, 50 × 4.6 mm i.d.), followed by a Thermo Hypersil Gold C(18) column (1.9 μm particle size, 50 × 2.1 mm i.d.) and the Thermo Hypersil BDS C(18) column (2.4 μm particle size, 100 × 2.1 mm i.d.). All columns required a mobile phase containing 1 m ammonium acetate buffer, pH 5.16, with a mixture of acetonitrile and methanol as the organic modifiers for optimum resolution of the type I and III isomers, particularly for uroporphyrin I and III isomers. All UHPLC columns were suitable and superior to conventional HPLC columns packed with 5 μm average particle size materials for clinical sample analysis.     

The novel assay method for nicotine metabolism to cotinine using high performance liquid chromatography

Nicotine is the primary psychoactive component in tobacco. It is taken into the body by tobacco smoking, and mainly metabolized to cotinine in the hepatic cytochrme P450 (CYP) 2A6. The objective of this study was to develop a sensitive method for the determination of nicotine metabolism to cotinine using HPLC. The internal standard, trans-4'-carboxycotinine methyl ester was synthesized with a simple method. The nicotine and cotinine were separated completely and detected by C(18) 5-μm analytical column (L-column Octa decyl silyl (ODS), 150 mm × 4.6 mm i.d.) equipped with a C(18) 5-μm guard column (L-column ODS, 10 mm × 4.6 mm i.d.) and ultraviolet detection at 260 nm. The detection limit of the assay was 0.05 μM for cotinine (n=5, R.S.D) and 0.1 μM for nicotine. Thus the present results provided a sensitive and useful method for the determination of nicotine metabolism catalyzed by CYP2A6.     

微流蒸发光散射检测器的研制及评价

构建了适用于纳升级到微升级流量的毛细管分离体系的微流蒸发光散射检测器(μELSD),实现了其与毛细管液相色谱(eLC)的联用.对雾化器孔径和雾化毛细管内径、蒸发管内径和长度、光散射池尺寸、雾化毛细管位置和辅助载气流量等参数进行了优化.在最优条件下,微流蒸发光散射检测器检出限为直接进样葡萄糖1 ng(S/N＞ 10),线性范围0.01～1.0 μg,重复性好,峰面积RSD(n=6)为0.4％,峰高RSD(n=6)为0.3％.本检测器已成功应用cLC-μELSD平台,使用C18毛细管色谱柱(内径250 μm),0.1％甲酸铵溶液(pH 4.5)-甲醇(60∶40,V/V)为流动相,分离检测了3种常用甜味剂,表明本研究构建的系统可以应用于实际分离检测中,具有分析时间快、溶剂消耗量少、样品需求量小的优点.     

Effect of monomer mixture composition on structure and chromatographic properties of poly(divinylbenzene-co-ethylvinylbenzene-co-2-hydroxyethyl methacrylate) monolithic rod columns for separation of small molecules

Porous poly(divinylbenzene-co-ethylvinylbenzene-co-2-hydroxyethyl methacrylate) monoliths were synthesized via thermally initiated free-radical polymerization in confines of surface-vinylized glass columns (150 mm × 3 mm i.d.) and applied to the reversed-phase separation of low-molecular-weight aromatic compounds. In order to compensate for the polymer shrinkage during the synthesis and prevent the monolith from detachment from the column wall, polymerization was conducted under nitrogen pressure. The reaction proceeded at 60°C for 22 h. 2,2'-Azo-bis-isobutironitrile was used as the initiator and 1-dodecanol was used as the porogen. A series of monoliths with different monomer ratios were obtained. All the monoliths had high specific surface areas ranging from 370 to 490 m(2)/g. In the studied range of monomer mixture compositions, the mechanical stability of the stationary phase in water/acetonitrile eluents was found to be high enough and practically insensitive to the fraction of 2-hydroxyethyl methacrylate (HEMA). Increasing the molar fraction of HEMA from 10.5% to 14.7% resulted in the decrease of column permeability by two orders of magnitude (from 1.1×10(-12) to 1.8×10(-14) m(2)) and led to weaker retention of alkylbenzenes. The higher HEMA content was shown to reduce the plate height of the columns in the separation of small molecules from 160-490 μm to 40-76 μm. This was attributed mainly to the decrease of the domain size of the monoliths leading to lower eddy dispersion and mass transfer resistance in the column.     

高效液相色谱-柱后化学发光法检测人体尿液中的卡托普利

在酸性条件下,Ce?氧化Ru(bipy)32+生成Ru(bipy)33+,同时氧化卡托普利生成二硫化物中间活性态([RS-SR]*),Ru(bipy)33+和二硫化物中间活性态之间相互反应产生强烈的化学发光。基于此,根据发光试剂Ru(bipy)32+水溶性好、试剂稳定等特点,将其加入到流动相中,通过高效液相色谱分离,建立了柱后化学发光快速灵敏检测卡托普利的方法。在以甲醇-0.01mol/L KH2PO4-1g/L Ru(bipy)32+(80∶20∶2,V/V)为流动相,流速为0.9mL/min,8.0×10-4 mol/L Ce?的优化实验条件下,方法的线性范围为2.0×10-7～1.0×10-4 mol/L(R2=0.9988),检出限为6.0×10-8 mol/L(S/N=3),并对1×10-5 mol/L卡托普利平行测定11次,相对标准偏差(RSD)为1.8%。将本方法用于人体尿液中卡托普利含量的测定,结果令人满意。结合化学发光光谱,对该体系发光机理进行了探讨。     

超临界流体色谱法分析非对映异构体d4T-5’-N-磷酰化苯丙氨酸甲酯

采用超临界CO2流体色谱技术,分析d4T-5’-N-磷酰化苯丙氨酸甲酯手性磷的非对映异构体。色谱柱为Hpersil ODS2(250 mm×4.6 mm,5μm),流动相为夹带改性剂甲醇、乙醇和异丙醇的超临界CO2流体。以容量因子、选择性和分离度为指标,考察改性剂、背压和柱温对分离的影响。在甲醇、乙醇和异丙醇3种改性剂中,甲醇为最好的改性剂,其中在7%甲醇改性剂下,该化合物的分离度可达到3.35。在7%甲醇改性剂条件下,考察了压力(10～20 MPa)和温度(303.15～318.15 K)的影响。在优化的分离条件(改性剂为7%甲醇,流速为2 mL/min,柱温为308.15 K,背压为15 M Pa)下,d4T-5’-N-磷酰化苯丙氨酸甲酯的两种非对映异构体完全达到基线分离,分离时间约15 min。     

对土壤及玉米植株中均三氮苯类除草剂的残留分析

土壤或玉米植株样品用Ｖ（甲醇）∶Ｖ（乙腈）＝１∶１提取,提取液用石油醚净化后,浓缩液过Ｃ１８小柱净化,最后用Ｎｏｖａ－ＰａｋＣ１８柱进行ＨＰＬＣ分析。回收率：氰草津为８２．４％～９９．８％,莠去津为８５．６％～１０２．３％,西草净为８９．１％～１０８．４％。