含氧阴离子的离子色谱法研究

 在含有阴、阳离子双官能团的色谱柱上 ,用两种浓度的Na2 HPO4洗脱液分别同时分离了 5种和 7种含氧阴离子 ,并且实现了元素不同价态的分析。 7.5mmol/LNa2 HPO4( pH 9.3)适于同时分离SeO32 - ,HAsO42 - ,SeO42 - ,WO42 - ,MoO42 - ,GeO32 - 和CrO42 - ;0 .75mmol/LNa2 HPO4(pH 9.3)适于同时分离IO3- ,H2 AsO3- ,BrO3- ,NO2 - 和NO3- ;检测波长为 2 0 4nm。另外 ,选择其它 4种阴离子色谱柱进行比较 ,对分离机理进行了初步的研究。     

化妆品中阴阳离子的快速测定及其用于化妆品鉴别的研究

用离子色谱电导检测器对黑泥类化妆品中的阴、阳离子(Na+,NH+4,K+,Mg 2+ ,Ca 2+ ,Cl-,Br-,NO-2,NO-3和SO 2- 4)进行了测定。阳离子分离条件: 阳离子交换柱ICS C25,均苯四甲酸淋洗液浓度2.0 mmol/L ,流速0.6 mL/min ;阴离子分离条件: 阴离子交换柱Shim pack IC A1,淋洗液为2.5 mmol/L 邻苯二甲酸和2.4 mmol/L 三羟基氨基甲烷,流速1.0 mL/min 。结果表明,上述10种离子在较宽浓度范围内有良好     

毛细管区带电泳技术快速分离检测爆炸残留物中的无机离子

利用间接紫外毛细管区带电泳方法完成了对爆炸残留物中7种无机离子(K+,NH+4,NO-2,NO-3,SO2-4,ClO-3,ClO-4)的分离检测。阳离子测定采用的缓冲体系为10 mmol/L吡啶（pH 4.5）-3 mmol/L冠醚,K+和NH+4在2.6 min内达到基线分离,检出限分别为0.25 mg/L和0.10 mg/L(S/N=3)。阴离子测定采用的缓冲体系为40 mmol/L硼酸-1.8 mmol/L重铬酸钾-2 mmol/L硼酸钠（pH 8.6）,氢氧化四甲铵为电渗流改性剂,5种阴离子在4.6 min内达到基线分离,检出限为0.10～1.85 mg/L。该方法已成功地应用于实际爆炸物样品种类的判定分析,取得了很好的结果。     

毛细管区带电泳技术快速分离检测爆炸残留物中的无机离子

利用间接紫外毛细管区带电泳方法完成了对爆炸残留物中7种无机离子(K+,NH+4,NO-2,NO-3,SO2-4,ClO-3,ClO-4)的分离检测。阳离子测定采用的缓冲体系为10 mmol/L吡啶（pH 4.5）-3 mmol/L冠醚,K+和NH+4在2.6 min内达到基线分离,检出限分别为0.25 mg/L和0.10 mg/L(S/N=3)。阴离子测定采用的缓冲体系为40 mmol/L硼酸-1.8 mmol/L重铬酸钾-2 mmol/L硼酸钠（pH 8.6）,氢氧化四甲铵为电渗流改性剂,5种阴离子在4.6 min内达到基线分离,检出限为0.10～1.85 mg/L。该方法已成功地应用于实际爆炸物样品种类的判定分析,取得了很好的结果。     

亲水单分散聚合物基质强阴离子色谱固定相的制备及应用

以自合成6.0μm大孔单分散交联聚甲基丙烯酸环氧丙酯微球为基质,采用化学键合法制备了季铵型强阴离子色谱填料,该填料具有良好的色谱性能。选用6.0 mmol/L Na2CO3+5.5 mmol/L NaHCO3混合液作淋洗液,在流速为1.0 mL/min下,可以很好地分离常见的6种无机阴离子(F-、Cl-、NO-2、Br-、NO-3、SO2-4)、4种低碳链酸(甲酸、乙酸、一氯乙酸、草酸)以及甲酸、乙酸和一些无机阴离子的混合物。考察了淋洗液种类、pH值和有机溶剂对6种无机阴离子分离的影响。在最佳色谱条件下,6种无机阴离子在一定浓度范围内具有良好的线性关系和低的检出限。采用该方法对本地自来水进行测定,4种离子可在22 min内完全分离,各离子的加标回收率为96.4%~100.6%。     

离子交换色谱法检测离子液体中阴离子

建立了用阴离子交换分离柱、化学抑制模式、电导检测测定系列离子液体中BF-4阴离子及其他杂阴离子(F-、Cl-、Br-)含量的方法,并用于在线监控离子液体合成工艺中阴离子杂质含量.确定淋洗液组成为1.6 mmol/L Na2CO3+3.9 mmol/L NaHCO3,流速为0.6 mL/min.本方法对所测阴离子检出限分别为50 μg/L(F-、Br-)和80 μg/L(BF-4);线性范围在3个数量级以上;r＞0.999;回收率在98%～102%之间.方法用于对离子液体小试工艺样品分析及过程监控时,结果满意,样品的RSD小于2.6%(n＝6).     

多孔单分散交联聚苯乙烯-二乙烯苯离子对色谱固定相分离8种阴离子

以一步种子溶胀聚合法制备的粒径为8 μm的多孔单分散交联聚苯乙烯-二乙烯苯(PSt-DVB)树脂为离子对色谱固定相, 2 mmol/L 氢氧化四丁基铵(TBAOH)、10%(V/V)乙腈和1.5 mmol/L Na2CO3的混合液为流动相, 在流速为1.0 mL/min下, 成功实现了8种阴离子(F-, Ac-, Cl-, NO-2, Br-, NO-3, SO2-4和HPO2-4)的分离.考察了淋洗液的配比对8种无机阴离子分离的影响.在最优条件下, 8种离子表现出良好的重现性及较好的线性关系, 色谱柱具有良好稳定性及较好的分离能力.将其用于雪水中阴离子的分析, 6种离子在15 min内完全分离, 各离子加标回收率在93.6%～110.4%之间.此固定相也可用于IO-3, HCOO-, ClO-3, BrO-3, ClCH2COO-和H2C2O4混合样的分离.     

黑火药余烬中无机阴离子的毛细管电泳方法研究

 发展了一种用于黑火药余烬中无机阴离子测定的毛细管电泳分析方法。对缓冲溶液的组成及pH值、电渗流改性剂的浓度以及分离电压等条件进行了研究。选定条件 :分离电压为 - 2 0kV ,缓冲溶液为 5 0mmol/L的Na2 CrO4(pH 8 2 0 ) ,电渗流改性剂为 0 5mmol/L的溴化十六烷基三甲基铵 (CTAB) ,检测波长为 2 5 4nm。在上述条件下 ,5种阴离子在 4min内可完全分离。各组分迁移时间和峰面积的相对标准偏差 (RSD)分别为 0 17%～1 4 0 %和 3 9%～ 5 0 % ,最低检测限为 5 0 μmol/L～ 10 0 μmol/L。     

离子色谱法测定浓磷酸中的Cl~–,SO_4~(2–),NO_3~–

采用离子色谱法测定浓磷酸中的Cl~–,SO_4~(2–),NO_3~–。将浓磷酸稀释至400倍体积,以0.22μm滤膜过滤,使用阴离子交换色谱–抑制电导检测器测定浓磷酸中的Cl~–,SO_4~(2–),NO_3~–。采用高容量色谱柱,以1.0 mmol/L Na_2CO_3–24 mmol/L Na OH混合液为流动相,将无机阴离子与浓磷酸基体分离,以标准加入法定量。氯离子、硝酸盐、硫酸盐的检出限为0.05~0.12 mg/L,加标回收率为96.6%~100.0%,测定结果的相对标准偏差为7.0%~10.0%(n=5)。该方法分离效果好,可用于浓磷酸中Cl~–,SO_4~(2–),NO_3~–的同时测定。     

离子色谱法同时测定饮水中9种阴离子

建立离子色谱抑制电导检测法同时测定饮水中F^-、Cl O₂^-、Cl^-、NO₂^-、Cl O₃^-、Br^-、NO₃^-、H₂PO₄^-和SO₄^2-9种阴离子的方法。采用SH-AP-2型阴离子交换柱为分离柱，以4.0 mmol/L Na₂CO₃-4.0 mmol/L Na HCO₃溶液为淋洗液，流量为0.80 m L/min，采用等度洗脱方式将9种阴离子完全分离，利用抑制电导检测。Cl O₂^-、Cl O₃^-的质量浓度在0.05～2.0 mg/L范围内，SO₄^2-     

蜂蜜中残留抗生素的填充毛细管液相色谱法检测

采用新型毛细管高效液相色谱法和自行填充的毛细管色谱柱,以四环素、土霉素和金霉素为标准物,对蜂蜜中残留的四环素类抗生素进行了定量分析。方法具有操作简单、灵敏度高、定量准确的优点。在10μg/L至0.4mg/L的质量浓度范围内,土霉素、四环素和金霉素的线性相关系数分别为rOTC=0.99695,rTC=0.99778和rCTC=0.98836。毛细管高效液相色谱法可用于抗生素类物质的高灵敏度测定。     

High-speed analyses using rapid resolution liquid chromatography on 1.8-microm porous particles

The potential of high-speed analyses by rapid resolution liquid chromatography (RRLC) and RRLC/MS on 1.8-microm porous particles packed into short columns operated at high flow-rate was investigated and compared with the performance of 5-microm porous particles packed into conventional columns. Using similar chemistries, the ease of conversion from conventional HPLC to an RRLC method was demonstrated. In order to display the practicality of RRLC separations, the analysis of pesticides in crops and catechins in Japanese green tea was selected. Using the Japanese Food Hygiene Law method, which employs a conventional 5-microm RP column (250 mm x 4.6 mm) for quantification of pesticides in crops, the analysis time was 25 min under isocratic conditions. Using the RRLC method on the short (50 mm x 4.6 mm) column packed with 1.8-microm porous particles, the same separation could be performed in 0.8 min with the RRLC/MS method without a loss in resolution. At the highest flow rate, compared to the conventional method, the time could be reduced by a factor of 31. In gradient elution, the fastest separation of catechins in Japanese green tea was achieved by RRLC on 50-mm x 4.6-mm id or 50-mm x 2.1-mm id RRLC columns packed with 1.8-microm particles. The analysis time at 5 mL/min was less than 1 min. Compared to the conventional HPLC method on a 150-mm column packed with 5-microm particles, time was reduced by a factor of 15. The effect of other experimental parameters such as the column temperature, acquisition rate of the detector and the influence of cell volume on chromatographic performance was also investigated. After the optimization, the analysis precision under the fastest RRLC conditions was examined. RSDs of retention time and peak area were 0.2% and 0.47%, respectively.     

Investigating the effects of protein patterns on microorganism identification by high-performance liquid chromatography-mass spectrometry and protein database searches

A method based on liquid chromatography coupled to mass spectrometry with positive electrospray ionisation was developed for the analysis of cyanobacterial hepatotoxins in environmental samples. The chromatographic separation was performed using two microbore columns, 2 mm and 1 mm I.D. columns, which allowed the coupling of liquid chromatography to mass spectrometry with no flow splitting. Analytes were eluted using two different water-acetonitrile, both acidified with formic acid gradients. Mass spectrometric parameters were optimised in order to maximise sensitivity. Detection limits for the 2 mm I.D. column ranged from 0.077 to 2.057 ng in full scan and from 0.021 to 1.153 ng in SIM mode. However, limits of detection as low as 60-340 pg in full scan and 6-72 pg in SIM mode were achieved for the 1 mm I.D. column. Finally, the proposed method was applied to the analysis of microcystins and nodularins in real samples.     

Analytical method for determination of disaccharides derived from keratan sulfates in human serum and plasma by high-performance liquid chromatography/turbo-ionspray ionization tandem mass spectrometry

We established a highly sensitive LC/MS/MS method for the analysis of the disaccharides produced from keratan sulfates (KS). It was revealed that the disaccharides produced by keratanase II enzymatic digestion of KS could be determined with high sensitivity by negative ion mode of multiple reaction monitoring. Furthermore, monosulfated and disulfated disaccharides can be separated using a Hypercarb (2.0 mm i.d. x 150 mm, 5 microm) with a gradient elution of acetonitrile-0.01 m ammonium bicarbonate (pH 10). This method was applied to the determination of KS in serum and plasma of control subjects. The intra-day precision expressed as %CV was within 6.8% for five replicate analyses with three different control serum. The inter-day (overall, n = 15) precision was within 7.3% for three days. This method is sensitive, reproducible and would be useful for clinical analysis.     

离子色谱法测定蔬菜硝酸盐含量

建立了化学抑制电导检测离子色谱法定性定量分析蔬菜硝酸盐含量的方法。阴离子分离柱DionexAS14柱(4mm×250mm),保护柱IonPacAG14(4mm×50mm)。流动相为1.7mmol.L-1NaHCO3,1.8mmol.L-1Na2CO3。流速1.2mL.min-1,自动连续再生抑制装置SRS-ULTRA4mm。线性范围为0.1~100.0mg.L-1,线性关系为0.9997,检出限为0.05mg.L-1。应用此法,测定了多种蔬菜硝酸盐含量。方法操作简单、快速、基体干扰少、灵敏、准确。     

Analysis of sulthiame in serum by narrow-bore high-performance liquid chromatography. Comparison of direct sample injection with pre-column switching and extrelut extraction.

Two high-performance liquid chromatographic methods for the analysis of sulthiame in serum are described. In the first method direct injection of serum samples onto a 4 x 4 mm I.D. (C18, 25 microns) precolumn in a column-switching device was used. After a purge step, the adsorbed analytes were eluted onto a 250 x 3 mm I.D. (C18, 5 microns) narrow-bore column for chromatographic separation. In the second method the sample pretreatment was an Extrelut extraction with dichloromethane-propanol-2 (95:5). After evaporation of the solvents, the residue was dissolved in methanol. The chromatographic separation was carried out on the same analytical column as used in the column-switching method. Both sample pretreatment methods were compared with respect to their suitability of routine analysis of sera from patients also receiving other antiepileptic drugs.     

填充毛细管液相色谱-毛细管气相色谱在线联用分析八角茴香挥发油

首次将填充毛细管高效液相色谱-毛细管气相色谱在线联用技术(μ-HPLC-CGC)用于分离分析八角茴香果实的挥发油成分。液相色谱选用氰基分析柱(250 mm×0.32 mm i.d.),正己烷-乙腈-二氯甲烷(体积比为80∶8∶12)为流动相,对挥发油样品做族组分分离,得到的5个族组分被依次存放在多位储存接口内,然后不分流分别转入毛细管气相色谱仪做详细分析。气相色谱柱由10 m×0.53 mm i.d.保留间隔柱和30 m×0.53 mm i.d.×1.0 μm SE-54分析柱组成。采用了不分流柱内进样模     

川西獐牙菜与抱茎獐牙菜中GFDA2酮的高效液相色谱分析

采用反相高效液相色谱法同时分离和测定了龙胆科獐牙菜属的川西獐牙菜和抱茎獐牙菜中几种GFDA2酮的含量。色谱柱为Kromasil C 18 （250 mm×4.60 mm i.d., 5 μ m）,流动相为甲醇 0.1%的磷酸水溶液（体积比为 73∶27 ）,流速1 mL/min ,检测波长260 nm,柱温20 ℃。实验结果表明,该方法具有很好的线性关系与精密度,方法简单、准确、实用性强。     

Direct injection versus liquid-liquid extraction for plasma sample analysis by high performance liquid chromatography with tandem mass spectrometry.

Direct injection versus liquid-liquid extraction for post-dose human plasma sample analysis by high performance liquid chromatography with tandem mass spectrometry (LC/MS/MS) have been studied using a drug candidate compound. For the direct-injection method, an Oasis(R) HLB column (1 x 50 mm, 30 micrometer) was used as the on-line extraction column and a conventional Waters symmetry C18 column (3.9 x 50 mm, 5 micrometer) was used as the analytical column. Each plasma sample (100 microL) was mixed with 100 microL of a working solution of the internal standard in aqueous 0.05 M ammonium acetate (pH 6.9), and portions (10 microL) of these samples were then injected into the LC/MS/MS system. For the liquid-liquid extraction method, a YMC Basic C18 column (2.0 x 50 mm, 5 micrometer) was used as the analytical column. Each sample (0.5 mL) was extracted with methyl tert-butyl ether and the extract was reconstituted and injected into the LC/MS/MS system. The total analysis time for both methods was 2.0 min per sample. The accuracy, inter-day precision and intra-day precision obtained from the quality control samples were within 8% for both methods. The analysis results of post-dose human plasma samples showed that the deviations of 91% of the concentrations obtained using the direct-injection method were within +/-20% from the concentrations obtained using the liquid-liquid extraction method, and the overall average percentage deviation was -1.5%. The results showed that the two methods were equivalent in terms of total chromatographic run time, accuracy and precision. However, for a batch of 100 samples, the sample preparation time for the direct-injection method was only about 25% of the time required for liquid-liquid extraction. This decrease in sample preparation time resulted in the doubling of the overall sample analysis throughput.     

Qualitative and quantitative determination of the major coumarins in Zushima by high performance liquid chromatography with diode array detector and mass spectrometry

A method, high-performance liquid chromatography coupled with diode array and electrospray tandem mass spectrometry (HPLC-DAD-ESI-MS), was developed to qualitatively identify and quantitatively determine the 10 major active coumarins of Zushima. The analysis was performed by using a ZORBAX SB-C18 analytical column (250 mm x 4.6 mm ID, 5 microm) at gradient elution of 0.5% aqueous formic acid and acetonitrile with diode array detection (325 nm). The method was validated for linearity, precision, accuracy, limit of detection and quantification. The proposed method was successfully applied for the qualitative and quantitative analysis of 10 coumarins in five different species of Zushima which had great variation on the contents of investigated coumarins.