固相萃取/高效液相色谱法测定水体中的戊唑醇

首次建立了固相萃取(SPE)-高效液相色谱法(HPLC)检测水中戊唑醇的方法并优化了固相萃取和高效液相色谱的条件.此方法对戊唑醇的检出限为0.01 μg/L,平均回收率为95.2%,相对标准偏差(RSD)为3.6%,线性范围为0.1～10 mg/L.应用该法分析了排放的废水和地表水,取得满意结果.     

离子交换固相萃取-液相色谱联用测定牛奶中的三聚氰胺

本文以混合型阳离子(MCX)固相萃取(SPE)小柱分离富集了牛奶提取液中的三聚氰胺,优化了固相萃取条件,复杂基质被有效去除,应用高效液相色谱(HPLC)法成功实现牛奶中三聚氰胺的检测,加标回收率接近90%。     

固相萃取—高效液相色谱法测定环境水体中的三环唑

建立了固相萃取—高效液相色谱法测定环境水体中三环唑的方法,在0.01mg/L～5.0 mg/L范围内线性关系良好,检出限为0.002mg/L,变异系数为2.5%,平均回收率为99.54%。     

分散固相萃取超高效液相色谱法快速测定水果中的杀菌剂残留

建立了散固相萃取超高效液相色谱法快速测定水果中的苯并咪唑类杀菌剂残留的分析方法.样品经乙腈提取后,均质离心,取上清液加入100 mg PSA及300 mg无水硫酸镁净化,离心取上清液进超高效液相色谱进行分析.对不同的色谱柱进行了选择性实验,最终采用C18柱,同时对流动相体系及净化条件进行了优化.结果：多菌灵、硫菌灵、噻菌灵、甲基硫菌灵在各自的浓度范围内呈良好的线性关系.对上述四种杀菌剂分别做3组（n=6）浓度水平的加标回收实验,平均回收率在80 ％～100％之间,相对标准偏差（RSD）均小于4.41％,四种杀菌剂的检出限（LOD）分别为多菌灵、噻菌灵0.1 mg/kg,硫菌灵、甲基硫菌灵0.05 mg/kg.实验结果表明,该方法简便、快速,适合水果中残留四种杀菌剂的测定.     

固相萃取技术富集水中酚类的影响因素探讨

采用固相萃取—高效色谱法测定水中酚类.通过正交实验和验证试验探讨固相萃取技术富集水中7种酚类各种因素的影响,优化固相萃取的条件.优化得到的固相萃取条件为：样品pH为2,选择Oasis HLB固相萃取色谱小柱,流速为：5 mL/min,洗脱溶剂为四氢呋喃,洗脱体积为2mL,分2次洗脱.所建立的方法具有回收率高、操作简便、溶剂用量少的特点.     

固相萃取-高效液相色谱法测定水中氯酚类

采用固相萃取-高效色谱法测定水中酚类。通过正交试验和验证试验探讨固相萃取技术富集水中7种酚类各种因素的影响,优化固相萃取的条件。优化得到的固相萃取条件：样品的pH为2、选择Oasis HLB固相萃取色谱小柱、流速为5mL／min、洗脱溶剂为四氢呋喃、洗脱体积为2mL,分2次洗脱。使用该方法的加标回收率为94．2％～105．1％,相对标准偏差为1．2％～3．9％,检出限为0．1～0．5μg／L。固相萃取-高效液相色谱法不仅各组分的回收率和灵敏度高,而且具有操作简便、溶剂用量少的特点,符合水中酚类测定的要求。     

固相萃取-高效液相色谱法测定食品中胭脂红酸含量

建立了食品中胭脂红酸含量的液相色谱测定方法。样品采用2 mmol/L HCl-甲醇提取,PLS固相萃取柱浓缩净化,以C18为色谱柱填料,以甲醇-0. 3%甲酸水体系为流动性进行色谱分离,在280 nm处进行测定。质量浓度在1～50μg/mL呈线性;方法回收率在85%～92%,相对标准偏差(n=6)均小于3%;该方法前处理简单、快速、准确,适合各类食品中胭脂红酸含量的测定。     

固相微萃取在食品安全检验中的应用

固相微萃取(SPME)技术是在固相萃取(SPE)的基础上发展出起来的一种新型样品前处理技术,它集采样、萃取、浓缩、进样于一体,可与GC、HPLC联用,检测简便、快速、无有机溶剂、选择性好、灵敏度高.本文介绍其装置、原理、SPME-GC联用技术、SPME-HPLC联用技术,及其在食品安全检验中的应用.     

水中酚类污染物的固相萃取富集与液相色谱分析

优化了水中酚类污染物的液相色谱操作条件,使１１种酚获得基线分离、灵敏检测。同时对固相萃取水中１０－９ｇ以下的酚类化合物的检测方法进行了评价。     

固相萃取-高效液相色谱法测定化妆品中的丙烯酰胺

建立了保湿防晒系列化妆品中丙烯酰胺含量的高效液相色谱测定方法.采用丙酮超声提取样品中的待测物,提取液经浓缩吹干后用水溶解,经固相萃取小柱净化后用反相高效液相色谱法测定.丙烯酰胺在0.01 mg/L～5.0 mg/L与对应峰面积呈良好线性关系(R=0.999 5).在添加量为0.05 mg/kg,0.50 mg/kg和1.00 mg/kg时,平均回收率在81.3%～83.8%,变异系数在2.3%～3.0%,方法检出限为0.05 mg/kg.结果表明,该法操作简便、灵敏、准确,适用于化妆品中丙烯酰胺含量的测定.     

高效液相色谱测定水中微囊藻毒素-LR的方法改进

采用C18固相苹取法预处理富集,纯甲醇作为洗脱剂,用液相色谱仪同时对水中的微囊藻毒素进行了测定。该方法简便、经济,节省了萃取剂的用量,减少了样品的预处理时间,具有较好的灵敏度、准确度和精密度,最低检测浓度为0-05mg／L,回收率达90%以上。     

Effect of absorbent in solid‐phase extraction on quantification of phospholipids in palm‐pressed fiber

Palm‐pressed fiber (PPF) is a by‐product of palm oil milling and it has been found to contain a high percentage of phospholipids (PL). The aim of this work was to evaluate the best solid‐phase extraction (SPE) method to purify PL from PPF. The purified PL were analyzed using high‐performance liquid chromatography (HPLC) with an evaporative light‐scattering detector (ELSD). The oil was extracted from PPF using the Folch method and classes of PL were purified using SPE. Different solvent phases and normal‐phase SPE cartridges [silica (Si), aminopropyl‐bonded silica (NH₂) and diol‐bonded silica (2OH)] at the same ratio of oil to sorbent mass were used to study the separation of PL from the extracted oil. The recovery of each standard PL was performed in a model oil system with the same amount of standard PL being added, and the repeatability of the SPE method was investigated. The isolation of PL by SPE diol cartridge and subsequent analysis by HPLC/ELSD have shown to be an accurate and reproducible analytical method for the determination of phosphatidylethanolamine, phosphatidylglycerol, phosphatidylcholine and lysophosphatidylcholine in PPF. This method provided a high yield and rapid separation of PL in PPF with less contamination from other lipid groups.     

Development trend and prospect of solid phase extraction technology

Solid phase extraction is widely used in sample pretreatment, concentration and analysis processes due to high selectivity and suitability for low concentration sample system. In this review, we systematically summarized and discussed the development trends of solid phase extraction by bibliometrics method. By analyzing papers output scale, the research and development direction of solid phase extraction technology is prospected. We also give an overview on current strategies of novel solid phase extraction from the separation medium and separation technology. The paper aims to describe the global research profile and the development trends of solid phase extraction, to help researchers to accurately grasp the research trend and to provide support for scientific research institutions to formulate scientific policies and strategic plans. Furthermore, the prospect of the development and application of solid phase extraction is also discussed.     

Analysis of fatty acid profile in plasma phospholipids by solid‐phase extraction in combination with GC

Phospholipids are recognised as an important source and transport form for metabolically active fatty acids. Therefore, detailed analysis of fatty acid profiles in plasma phospholipids as marker for dietary habits or interventions gains more and more importance. Appropriate analytical methods described so far are either expensive or susceptible to handling errors. We developed a method to separate plasma phospholipids by acetone fractionation combined with SPE in order to analyse the fatty acid compositions in phospholipid fractions of human plasma by GC analysis. The method has been validated in order to be applied to the routinely performed analysis of the samples of patients who will be participating in a dietary supplement study. The method presented here was successfully validated and is stable, efficient and reproducible. It can be used in a routine fashion to deliver the fatty acid profile [palmitic acid (16:0), heptadecanoic acid (17:0), stearic acid (18:0), oleic acid (18:1n‐9), linoleic acid (18:2n‐6), linolenic acid (18:3n‐3), arachidonic acid (20:4n‐6), eicosapentaenoic acid (20:5n‐3) and docosahexaenoic acid (22:6n‐3)] in plasma phospholipid samples. Using a sample volume of 500 µL, recovery of plasma phospholipids is 92 ± 11%; LOQ is 2.2 µg fatty acid/mL. A set of samples from cancer patients and healthy individuals was analysed and confirmed the applicability of the described method.     

对甲苯磺酸的高效液相色谱分析

建立了高效液相色谱测定对甲苯磺酸纯度的方法.色谱柱为ODS柱;流动相为水-乙腈-磷酸溶液(体积比为46.7:53.15:0.15),流速0.8 mL/min;紫外检测波长为254 nm;柱温为30 ℃;对甲苯磺酸的质量浓度为22.62～362.00 mg/L时,峰面积与质量浓度具有良好的线性关系,相关系数为0.999 ...     

PVC玩具中壬基酚的分子印迹基质固相分散-超高效液相色谱法测定

以对模板分子具有较强识别特性的分子印迹聚合物为基质固相分散吸附剂,提取PVC塑料玩具中的壬基酚,用超高效液相色谱法进行测定,研究壬基酚分子印迹聚合物对样品中壬基酚的提取和净化效果。结果表明:在优化条件下,该方法的检出限为0.13 ng/mL,定量限为0.47 ng/mL,不同壬基酚添加量的回收率93.5%,相对标准偏差3.4%。此方法分离效果好、灵敏度高,适用于PVC玩具中壬基酚的测定。     

固相萃取技术的应用与研究新进展

固相萃取技术(SPE)是近年来发展较快并得到广泛应用的一种新前处理方法,介绍了固相萃取技术的基本原理及方法。对固相萃取技术在食品、药品、和环境检测等领域的应用进行了综述,阐述了目前对固相萃取技术的研究开发和发展展望。     

固相萃取气相色谱法测定水中的溴氰菊酯

采用C18固相萃取法预处理富集，石油醚作为洗脱剂，用气相色谱仪对水中的浚氰菊酯进行了测定。该方法简便，经济，节省了萃取剂的用量，减少了样品的用量和预处理时间，具有较好的灵敏度、准确度和精密度，最低检测浓度为0．1μg/L，回收率达83％以上。     

Determination of sulfonylurea herbicides in soil samples via supercritical fluid extraction followed by nanostructured supramolecular solvent microextraction

The present work describes a sensitive procedure for extraction and determination of three sulfonylurea herbicides (metsulfuron-methyl, bensulfuron-methyl and chlorsulfuron) in water samples using supramolecular solvent microextraction. A supramolecular solvent with a nano structure made up of decanoic acid assemblies dispersed in tetrahydrofuran and water was proposed. Also, a supercritical fluid extraction coupled with supramolecular solvent microextraction was applied for extraction and determination of ultra-trace amounts of sulfonylurea herbicides in soil samples. A Taguchi orthogonal array experimental design with an OA₁₆ (4⁵) matrix was employed to optimize the supercritical fluid extraction conditions. In supercritical fluid extraction–supramolecular solvent microextraction procedure, a mixture of decanoic acid and the SFE collecting solvent (tetrahydrofuran) was added to water for supramolecular solvent formation. The effective parameters on the supramolecular solvent microextraction efficiency were studied and optimized using two different optimization methods: one variable at a time and face centered design. Under the optimum conditions, linear dynamic ranges varied within 0.1–5 mg kg⁻¹ (0.9978 ≤ R² ≤ 0.9987) and 0.5–100 μg L⁻¹ (0.9973 ≤ R² ≤ 0.9995) for all of the sulfonylurea herbicides in the supercritical fluid extraction–supramolecular solvent microextraction and supramolecular solvent microextraction, respectively. The intraday (n = 5) and interday standard deviations were calculated by extracting the SUHs from water and soil samples through supramolecular solvent microextraction and supercritical fluid extraction–supramolecular solvent microextraction. Interday RSDs% lower than 7.1% and intraday RSDs% lower than 3.8% were obtained. Limits of detection, based on a S/N ratio of 3, were 0.5 μg L⁻¹ and 0.7 mg kg⁻¹ for supramolecular solvent microextraction and supercritical fluid extraction–supramolecular solvent microextraction, respectively.