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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%。 相似文献
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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. 相似文献
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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. 相似文献
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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。 相似文献
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固相萃取-高效液相色谱法测定化妆品中的丙烯酰胺 总被引:2,自引:0,他引:2
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. 相似文献
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Seong Chea Chua Chin Ping Tan Oi Ming Lai Kamariah Long Hamed Mirhosseini Badlishah Sham Baharin 《European Journal of Lipid Science and Technology》2008,110(4):334-340
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. 相似文献
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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. 相似文献
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Lenka A. Taylor Vittorio Ziroli Ulrich Massing 《European Journal of Lipid Science and Technology》2009,111(9):912-919
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. 相似文献
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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. 相似文献