高效液相色谱法测定土壤中草甘膦的残留

通过优化色谱条件,建立了快速萃取—高效液相色谱法检测土壤中草甘膦的残留量.草甘膦在0.01 ～0.50 mg/L范围内线性关系良好,相关系数(R2) ＞0.999,检出限0.01 mg/kg;在土壤中加标0.100、0.500和1.00 mg/kg,草甘膦的平均加标回收率为80.0％ ～ 100％,相对标准偏差为5.3...     

高效液相色谱法测定土壤中丙烯酰胺的含量

建立高效液相色谱法测定土壤中丙烯酰胺的含量,样品经超声提取、离心、过滤等步骤,经ZORBAX Eclipse Plus C18色谱柱(4.6×100 mm,3.5μm)分离; V(甲醇)∶V(水)=5∶95为流动相,DAD检测器波长210 nm。方法在0.05～5.0μg/m L范围内与色谱峰面积线性关系良好,相关系数(r)不小于0.999。土壤中丙烯酰胺的检出限为0.02 mg/kg,加标回收率在77.1%～99.5%之间,测定结果的相对标准偏差均小于10%(n=6)。该方法适用于土壤中丙烯酰胺含量的检测。     

吹扫捕集气相色谱法测定水性涂料中的苯系物

建立了吹扫捕集气相色谱法测定水性涂料中8种苯系物的分析方法,对色谱条件、吹扫条件等进行了探讨,同时对分析参数如线性相关性、相对标准偏差、最低检出限及加标回收率进行了评价.结果表明:采用吹扫捕集气相色谱法,在2.5～ 50.0 μg/L范围内,8种苯系物的质量浓度和峰面积呈良好的线性关系;对加标浓度为5.0μg/L的涂料样品平行测定7次,其相对标准偏差为1.8％～4.3％;水性涂料样品的加标回收率在88.3％ ～ 107％之间;最低检出限在0.50～1.0 μg/L之间.     

高效液相色谱法测定洗发产品中5种违禁添加药物

建立了高效液相色谱法同时测定洗发产品中酮康唑、甲硝唑、氯霉素、丙酸氯倍他索及醋酸曲安奈德等5种违禁药物成分的方法.在SunFire-C(18)(5μm,4.6 mm×150 mm)色谱柱上,以甲醇和乙酸铵水溶液梯度洗脱,检测波长为254 nm,流速为1 mL/min,柱温为30℃.检出限为0.08 mg/L～0.20 mg/L,各组分在2.0 mg/L～50.0 mg/L呈良好线性关系,相关系数为0.999 5～0.999 9,样品加标回收率为89.2%～97.8%,相对标准偏差为1.56%～3.26%.     

高效液相色谱法测定简易塑料手套中邻苯二甲酸二丁酯的研究

建立了高效液相色谱法测定简易塑料手套中邻苯二甲酸二丁酯的分析方法。简易塑料手套需要一系列的处理后,提取后浓缩即可进样。实验的色谱条件,柱温35℃,流动相为甲醇,流速为1 m L/min,检测波长228 nm。结果表明,建立的方法在0.041 8⁰.627 0 mg/m L范围内具有良好的线性关系(r=0.999 0),方法的检出限(LOD)为0.418μg/m L;应用该方法测定简易塑料手套中的邻苯二甲酸二丁酯,实际样品的加标回收率在83.3%0.627 0 mg/m L范围内具有良好的线性关系(r=0.999 0),方法的检出限(LOD)为0.418μg/m L;应用该方法测定简易塑料手套中的邻苯二甲酸二丁酯,实际样品的加标回收率在83.3%¹05.7%,相对标准偏差(RSD%)低于2.23%。该方法操作简单、快速、准确,可用于不同塑料手套中塑化剂组分中邻苯二甲酸二丁酯的分析。     

高效液相色谱法测定化妆品中大麻二酚

建立了高效液相色谱法测定化妆品中大麻二酚的分析方法。采用ZORBAX Eclipse Plus C18柱(250 mm×4.6 mm,5 μm),流动相为磷酸二氢钠-甲醇混合溶液,流速1.0 mL/min,柱温25 ℃,检测波长220 nm,进样量10 μL。结果表明,大麻二酚在10～200 mg/L峰面积与质量浓度呈良好的线性关系,相关系数为0.999 9 (n=5),方法检出限为5 mg/kg;加标回收率为96.47%～101.23%,相对标准偏差为0.39%～1.48%(n=6)。该方法操作简便,具有良好的重复性和回收率,可用于化妆品中大麻二酚的检测。     

离子色谱法测定尿素中硫酸铵含量

建立离子色谱法测定尿素中硫酸铵含量的分析方法。该方法将尿素样品在250℃灼烧1 h后能分解80%的尿素且不影响硫酸根的稳定性,大大减少了有机物对色谱柱的污染,然后采用离子色谱仪测定样品中硫酸根离子浓度。硫酸根离子质量浓度在10～50 mg/L范围内线性良好,相关系数为0.999 8,方法检出限为0.001 mg/L,定量限为0.01 mg/L,测定结果的相对标准偏差为0.04%～0.05%(n=6),样品加标回收率为101.8%～104.7%。该方法能够将样品中大部分尿素除去,减少杂质的干扰,可用于尿素中硫酸根离子含量的测定。     

超高效液相色谱法测定稻田水和土壤中噻嗪酮的残留量

建立了超高效液相色谱法测定噻嗪酮在稻田水和稻田土的残留分析方法。田水样品经二氯甲烷液液萃取;土壤经甲醇提取,二氯甲烷萃取,UPLC测定,外标法定量。在0.209～41.8 mg/kg质量浓度范围内,仪器响应值与质量浓度呈良好线性关系(r>0.9999)。平均回收率为83.81%～104.4%,相对标准偏差为0.62%～10.78%;噻嗪酮在田水和土壤中的最小检出限分别为0.004 mg/kg和0.01 mg/kg。     

高效液相色谱法测定糖果中的酸性红

建立了高效液相色谱法测定糖果中酸性红的方法。酸性红在2.5～100.0μg/m L浓度范围内,峰面积与浓度呈良好的线性关系,Y=42418.3X+217.5(r=0.99997),检出限为0.5mg/kg,相对标准偏差小于5%,样品加标回收率范围98%～100%。该方法检测速度快、精密度和准确度较高,可用于糖果中酸性红含量的测定。     

高效液相色谱法测定化妆品中的肌肽含量

建立了高效液相色谱—二极管阵列检测器(HPLC-DAD)测定化妆品中肌肽含量的方法。样品在破乳剂存在的条件下,用纯水经超声波提取30 m i n,在3 000 r/m i n条件下离心1 0 m in,采用Prevail~(TM)Carbohydrate ES色谱柱(250 mm×4.6 mm,5μm),以甲醇与乙酸水溶液(pH 3.5)作为流动相,以1.0 mL/min进行等度洗脱,检测波长为210 nm,柱温25℃。结果显示,肌肽在0.2~20.0 mg/L呈良好的线性关系,相关系数为0.999 9,保留时间和峰面积的相对标准偏差均小于0.5%,加标回收率为93.33%~108.64%,检出限为0.02mg/L,定量限为0.07mg/L。     

High-Pressure Gas Chromatography and Chromatography with Supercritical Fluids. III. Fluid-Liquid Chromatography

Abstract

High-boiling substances can be separated by partition chromatography, using n-pentane and isopropanol under supercritical conditions as mobile carriers. At moderate temperatures (200–250°C) the volatility of heavy substances may be enhanced by a factor of as much as 10⁴ by increasing the pressure from atmospheric to about 50 kg/cm². This enables the analysis of compounds which are too heavy for ordinary gas chromatography.

As predicted before on the basis of gas-chromatographic studies at elevated pressures, the use of supercritical mobile fluids in combination with liquid stationary phases results in an attractive separation procedure. This technique is rapid and has a high degree of flexibility. Separations according to boiling point as well as molecular type are possible.

The main features of the new chromatographic technique, for which the designation “fluid-liquid chromatography” (FLC) is proposed, are illustrated by means of several examples.     

亲和色谱法

<正> 目前亲和色谱法已发展成为解离和纯化生物物质不可缺少的技术。在一般情况下,活跃细胞中的分离目的物,特别是高级有机物体,其浓度极低并与几千种相似物混在一起,亲和色谱法分离这些复杂混合物,远比利用物理性质渐次的差异,如组分的重量、大小、形状和溶解度等传统技术为优越。     

Particle Chromatography

Abstract

Particle mixtures can be separated into bands by slowly increasing the freezing rate during directional solidification. Continuous size classification of spherical particles can similarly be obtained.     

纸色谱和柱色谱实验方法的改良

对纸色谱和柱色谱实验的方法进行了改良,改良后的实验具有操作方便、现象明显、实验时间短、经济、环保的优点。     

Inverse Paper Chromatography

Abstract

Available methods of examination do not provide absolute certainty that two samples of paper have the same origin. A new technique for testing paper, known as inverse paper chromatography (IPC), is based on using a strip of paper as the chromatographic sorbent medium on which a mixture of known probes is separated under standardized conditions. The resulting chromatogram will uniquely designate the paper grade and composition. This principle has been validated with 36 types of paper in a standard test, using cresol red, chlorophenol red, bromothymol blue, fuchsine, and methylene blue as the probe mixture and n-butanol as the eluant. The machine direction in the paper is distinguishable by this method. The experimental technique is simple, inexpensive, and essentially nondestructive. Exposure of paper sheets to physical influences such as printing, wetting, humidity, and filtered sunlight does not alter their characteristic chromatographic behavior. However, baking (artificial aging) and exposure to direct sunlight change the chromatographic performance of the paper, evidently by inducing chemical changes. Incorporating colored pigments in the paper also alters the chromatographic separations obtained. The application of IPC to forensic science, product testing, and paper chemistry is discussed. A facile stiffness test for unequivocally determining the machine direction in a paper sheet is described that provides a technique for revealing fraudulent page insertion in a multipage document.     

Pressurized Continuous Chromatography

Abstract

A pressurized continuous annular chromatograph has been developed for preparative separations. This device utilizes a slowly rotating annular bed of sorbent material, fixed multiple feed points, and fixed withdrawal locations. Most of our investigations have been performed with a 28-cm-diam column, but a larger model is being designed and constructed. The separation of copper, nickel, and cobalt components from a carbonate solution has been studied in detail. This solution simulates the leach liquor from the Caron process for recovering nickel and cobalt from laterite ores. Use of continuous gradient elution has been demonstrated. Recent studies have investigated several separations, including that of zirconium and hafnium (necessary for the production of zirconium for use in nuclear reactors), on a preparative scale. This system, because of its continuous feed and product withdrawal, its adaptability to large-scale operations, and its ability to separate many components, is expected to make chromatography a more competitive process in the industrial sector.     

Gel Filtration Chromatography

Abstract

The technique of gel filtration chromatography is described, with a guide to relevant literature on methods, theory, and applications, especially the use of GFC in analysis of molecular interactions, both macromolecular and small molecule-macromolecule aggregation.