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雌激素类内分泌干扰物的液相色谱-质谱分析样品前处理方法 总被引:2,自引:1,他引:2
本文对液相色谱-质谱分析过程中雌激素的样品前处理方法进行论述,内容涉及环境雌激素的样品前处理方法和近年来的应用。引用文献77篇。 相似文献
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用于气相色谱和气相色谱-质谱测定植物样品中含氯有机污染物残留的样品前处理方法 总被引:3,自引:0,他引:3
根据植物样品中的主要干扰物质,建立了用于气相色谱(GC)和气相色谱-质谱联用(GC-MS)测定植物样品中含氯有机污染物残留的样品前处理方法,有效提高了对植物样品中有机氯农药及多氯联苯检测的灵敏度。采用均质提取法对样品进行提取,考察了凝胶渗透色谱(GPC)和固相萃取(SPE)对提取液的净化效果。结果发现,采用GC测定目标物时,提取液需经GPC和SPE两次净化;而采用GC-MS测定目标物时,仅用SPE一次净化即可。该方法快速、经济、灵敏,适合多种植物样品中有机污染物残留分析的样品前处理要求。 相似文献
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通过系统考察血清样本前处理方法、优化液相色谱条件及质谱检测参数,建立了脂质组学血清样本前处理及其快速高分辨液相色谱-质谱(RRLC-MS)分析方法。血清样本中加入二氯甲烷-甲醇(CH2Cl2-CH3OH,2∶1,V/V)混合溶剂进行脂质提取,采用ACQUITY UPLC CSH C18色谱柱(100 mm×2.1mm,1.7μm),以10 mmol/L甲酸铵溶液(含0.1%甲酸)为流动相A,乙腈-异丙醇(1∶1,V/V)为流动相B,梯度洗脱,采用正负离子检测模式电喷雾电离(±)ESI、正离子检测模式大气压化学电离(+)APCI方式进行质谱检测。对血清中脂肪酸、甘油脂、鞘磷脂、甘油磷脂和胆固醇(酯)5类14种代表性脂质类成分进行了方法学考察。结果表明,方法灵敏度高、精密度及稳定性良好。对穿插在检测序列中的质控样本检测结果进行主成分分析(PCA),证明了本方法获得数据的可靠性良好,适用于脂质组学研究。 相似文献
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Ling Xia Yanxia Li Yulan Liu Gongke Li Xiaohua Xiao 《Journal of separation science》2020,43(1):189-201
Sample preparation is the procedure before instrumental analysis and significant to its effectiveness and efficiency. However, this procedure is usually time‐consuming, labor intensive, and prone to error. In the last decade, the development of sample preparation techniques has received increasing attention, especially in complex sample application. To pretreat samples faster and more effectively, advanced materials, instrumentation, and methods have been combined with typical techniques, including extraction, membrane separation, and chemical conversion techniques. Researchers in China focused on the development of simple, efficient sample preparation methods with selective enrichment and rapid separation capabilities for target analysis in complicated sample matrix and contribute almost a half of the publications in this specific field. In this review, a panorama of sample preparation techniques in China has been composed from more than 140 references, and we highlight some promising methods developed during recent years and introduce different separation materials with respect to these methods. 相似文献
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Juliana Soares da Silva Burato Deyber Arley Vargas Medina Ana Lúcia de Toffoli Edvaldo Vasconcelos Soares Maciel Fernando Mauro Lanas 《Journal of separation science》2020,43(1):202-225
Advances in the area of sample preparation are significant and have been growing significantly in recent years. This initial step of the analysis is essential and must be carried out properly, consisting of a complicated procedure with multiple stages. Consequently, it corresponds to a potential source of errors and will determine, at the end of the process, either a satisfactory result or a fail. One of the advances in this field includes the miniaturization of extraction techniques based on the conventional sample preparation procedures such as liquid‐liquid extraction and solid‐phase extraction. These modern techniques have gained prominence in the face of traditional methods since they minimize the consumption of organic solvents and the sample volume. As another feature, it is possible to reuse the sorbents, and its coupling to chromatographic systems might be automated. The review will emphasize the main techniques based on liquid‐phase microextraction, as well as those based upon the use of sorbents. The first group includes currently popular techniques such as single drop microextraction, hollow fiber liquid‐phase microextraction, and dispersive liquid‐liquid microextraction. In the second group, solid‐phase microextraction techniques such as in‐tube solid‐phase microextraction, stir bar sorptive extraction, dispersive solid‐phase extraction, dispersive micro solid‐phase microextraction, and microextraction by packed sorbent are highlighted. These approaches, in common, aim the determination of analytes at low concentrations in complex matrices. This article describes some characteristics, recent advances, and trends on miniaturized sample preparation techniques, as well as their current applications in food, environmental, and bioanalysis fields. 相似文献
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Sample preparation turns out to be one of the important procedures in complex sample analysis by affecting the accuracy, selectivity, and sensitivity of analytical results. However, the majority of the conventional sample preparation techniques still suffer from time-consuming and labor-intensive operations. These shortcomings can be addressed by reforming the sample preparation process in a microfluidic manner. Inheriting the advantages of rapid, high efficiency, low consumption, and easy integration, microfluidic sample preparation techniques receive increasing attention, including microfluidic phases separation, microfluidic field-assisted extraction, microfluidic membrane separation, and microfluidic chemical conversion. This review overviews the progress of microfluidic sample preparation techniques in the last 3 years based on more than 100 references, we highlight the implementation of typical sample preparation methods in the formats of microfluidics. Furthermore, the challenges and outlooks of the application of microfluidic sample preparation techniques are discussed. 相似文献
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植物激素样品前处理方法的研究进展 总被引:1,自引:0,他引:1
植物激素是植物中一类含量很低,却对植物生长发育等生命过程起重要调控作用的有机化合物。近年色谱/质谱联用技术不断发展,已成为植物激素分析的常用方法,而样品前处理则是色谱分析过程中的一个关键环节,所以高选择性和高回收率的前处理方法对于植物激素的分析至关重要。根据植物激素的化学性质,本文将其分为酸碱性植物激素、油菜素甾醇、植物多肽3类,并对相应的前处理方法加以综述,特别是近年来发展起来的新方法。内容包括前处理方法的原理、装置、萃取材料以及衍生试剂等,相关内容主要围绕本研究组的痕量植物激素研究工作展开,最后对研究趋势做了简短展望。 相似文献
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样品前处理技术在样品分析中发挥着越来越重要的作用,而对分析物的富集能力和对样品基体的净化程度主要取决于高效的样品前处理材料,所以发展高性能的样品前处理材料一直是该领域的前沿研究方向。近年来,各类先进材料已经被引入样品前处理领域,发展了多种高性能的萃取材料。由于独特的物理化学性质,石墨烯已在各个研究领域获得广泛关注,在样品前处理领域也发挥着重要作用。基于高的比表面积、大的π电子结构、优异的吸附性能、丰富的官能团和易于化学改性等优点,石墨烯和氧化石墨烯基萃取材料被成功应用于各种样品的前处理,对不同领域中多种类型分析物表现出优异的萃取性能。该论文总结和讨论了近3年来石墨烯材料(石墨烯、氧化石墨烯及其功能化材料)在柱固相萃取、分散固相萃取、磁性固相萃取、搅拌棒萃取、纤维固相微萃取和管内固相微萃取等方面的研究进展。基于多种萃取机理如π-π、静电、疏水、亲水、氢键等相互作用,石墨烯萃取材料能够高效萃取和选择性富集不同类别的目标分析物,如重金属离子、多环芳烃、塑化剂、雌激素、药物分子、农药残留、兽药残留等。基于新型石墨烯萃取材料的各种样品前处理技术与多种检测技术如色谱、质谱、原子吸收光谱等联用,广泛应用于环境监测、食品安全和生化分析等领域。最后,总结了石墨烯在样品前处理领域中存在的问题,并展望了未来的发展趋势。 相似文献
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脂质不仅是细胞膜的主要组成部分,还参与一些生命活动如能量存储、信号传导等,在生命体中发挥着重要作用。近年来,越来越多的研究表明脂质的变化与一些重大疾病的发生发展密切相关,脂质组学研究对理解疾病的发生机制及过程具有重要意义。在脂质分析过程中,由于样品基质的干扰或被分析物浓度的限制,通常需要对样品进行前处理,以得到最佳的分析性能。该文综述了脂质组学分析中的样品前处理技术,包括脂质的提取方法(如液液萃取、固相萃取等)和针对不同类脂质的化学衍生化技术在各领域,尤其是生命分析和代谢组学中的应用,并对脂质组学分析中的样品前处理技术的发展进行了展望。 相似文献
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顶空气相色谱-质谱联用技术的应用进展 总被引:1,自引:0,他引:1
顶空分析作为一种无有机溶剂萃取的样品处理技术,通常与气相色谱-质谱(GC-MS)技术结合用来分析复杂基质中的挥发性有机物。顶空气相色谱-质谱(HS-GC-MS)技术具有快速、高效、环保、灵敏度高等特点,在常规分析中发挥着重要作用。该文简要概述了静态顶空、动态顶空、顶空固相微萃取分析以及GC-MS联用技术,并介绍了整个顶空分析系统的影响因素和优化过程。根据基质类型的分类,综述了HS-GC-MS在食品和饮料、环境、生物等样品中的应用实例。HS-GC-MS的研究非常活跃,不断出现新应用,在分析挥发性有机物方面具有广阔前景。 相似文献
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Application of ethyl chloroformate derivatization for gas chromatography-mass spectrometry based metabonomic profiling 总被引:2,自引:0,他引:2
A new combined gas chromatography and mass spectrometry (GC-MS) method has been developed suitable for the urine sample treatment in aqueous phase with ethyl chloroformate (ECF) derivatization agents. The method has been extensively optimized and validated over a broad range of different compounds and urine samples. Analysis of test metabolite derivatives, containing spiked standards, or rat urine exhibited acceptable linearity, satisfactory intra-batch precision (repeatability) and stability, relative standard deviations (R.S.D.) less than 10 and 15% within 48 h, respectively. The quantification limits were 150-300 pg on column for most metabolites. Recovery of several representative compounds, at different concentrations, ranged from 70 to 120%, with R.S.D. better than 10% for rat urine. We were able to generally eliminate potentially confounding variables such as medium complexity, different urea concentrations, and/or derivatization procedure variability. Metabonomic profiling of 1,2-dimethylhydrazine (DMH)-induced precancerous colon rat urine using GC-MS with ECF derivatization was performed to evaluate the proposed method. The analytical variation of the method was smaller than the biological variation in the rat urine samples, proving the suitability of the method to analyze differences in the metabonome of a living system with perturbed metabolic network. Thus, the proposed GC-MS analytical method is reliable to analyze a large variety of metabolites and can be used to investigate human pathology including disease onset, progression, and mortality. 相似文献
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Johanna Steen Margareta RamströmSophia Hober Jenny Ottosson 《Journal of chromatography. A》2009,1216(20):4457-4464
A completely automated procedure for the purification and desalting of proteins with a polyhistidine purification tag prior to mass spectrometry analysis is presented. The system is ideal for rapid quality control and optimization studies and it provides researchers with a straightforward, reliable tool for studies of recombinant proteins. Forty-eight samples can be prepared within 4.5 h and only small cultivation and buffer volumes are needed. In this proof of concept, 19,000–35,000 Da recombinant proteins from both crude and clarified cell lysates were successfully prepared for subsequent analysis by electrospray ionization and matrix-assisted laser desorption/ionization mass spectrometry as well as by gel electrophoresis. 相似文献