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同时亚临界水萃取与固相萃取从河流沉积物中分离有机氯化合物 被引量:4
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作者 黄卫红 李春香 +1 位作者 柳天舒 阎永胜 《理化检验(化学分册)》 CAS CSCD 北大核心 2007年第11期950-952,955,共4页
静态亚临界水萃取中加入固相萃取剂对河流沉积物中4种有机氯化合物(2-氯酚、2,4,6-三氯酚、五氯酚、六氯苯)进行了同时萃取。与离线亚临界水萃取-固相萃取方法相比,分析物的萃取回收率均有提高,且受亚临界水萃取罐冷却程度的影响较小。... 静态亚临界水萃取中加入固相萃取剂对河流沉积物中4种有机氯化合物(2-氯酚、2,4,6-三氯酚、五氯酚、六氯苯)进行了同时萃取。与离线亚临界水萃取-固相萃取方法相比,分析物的萃取回收率均有提高,且受亚临界水萃取罐冷却程度的影响较小。以活性炭纤维(ACF)为固相萃取剂,在160℃时,0.050 g的ACF和4.0 mL水对0.500 g的加标沉积物样品中的2-氯酚(2-CP),2,4,6-三氯酚(246-TCP),五氯酚(PCP)和六氯苯(HCB)的萃取效率比离线亚临界水萃取-固相萃取的回收率均有所提高,萃取回收率受萃取罐冷却温度影响较小。方法特别适合于高含量的沉积物样品萃取。该方法与气相色谱检测联用,分析了长江镇江段沉积物中4种有机氯化合物的含量,结果与美国环保署(USEPA)标准方法所得的结果吻合。 展开更多
关键词 同时亚临界水- 活性炭纤维 沉积物 有机氯污染物
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高效液相色谱法测定乳粉和鸡肉中5种性激素 被引量:3
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作者 郑永杰 靳凤龙 田景芝 《化学试剂》 CAS CSCD 北大核心 2013年第6期522-526,共5页
建立液液萃取(LLE)-固相萃取(SPE)-高效液相色谱(HPLC/DAD)方法对乳粉和鸡肉中5种性激素进行测定。实验采用LLE和SPE联合技术对复杂基质样品进行净化处理,优化了萃取过程中溶剂及固相萃取小柱种类。同时,采用反相C18色谱柱,梯度洗脱方... 建立液液萃取(LLE)-固相萃取(SPE)-高效液相色谱(HPLC/DAD)方法对乳粉和鸡肉中5种性激素进行测定。实验采用LLE和SPE联合技术对复杂基质样品进行净化处理,优化了萃取过程中溶剂及固相萃取小柱种类。同时,采用反相C18色谱柱,梯度洗脱方式进行色谱定性、定量分析。结果表明,目标分析物在1.0~200.0μg/mL范围内有良好的线性相关性,方法检出限4.7~21.0μg/kg,方法回收率88.8%~104.2%,相对标准偏差<7.2%。应用该方法对市质检所送检的10批次乳粉和鸡肉样品进行分析,5种性激素均未检出。该方法灵敏、可靠,显示出其富集与分离实际食品样品中多种性激素的良好应用前景。 展开更多
关键词 性激素 液液- 高效液色谱 乳粉 鸡肉
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海水中雪松醇的SPME-GC-MS测定及其与赤潮关系 被引量:2
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作者 赵明桥 李攻科 +1 位作者 陈皓 张展霞 《分析测试学报》 CAS CSCD 北大核心 2002年第6期5-8,共4页
建立了用固相微萃取 -气相色谱 -质谱联用测定海水中雪松醇的分析方法 ;优化了萃取涂层、萃取时间、萃取温度、搅拌速度、介质离子强度、解吸温度和时间等实验条件 ;方法的线性范围为0.020~10μg/L ,检出限为0.008μg/L,相对标准偏差在... 建立了用固相微萃取 -气相色谱 -质谱联用测定海水中雪松醇的分析方法 ;优化了萃取涂层、萃取时间、萃取温度、搅拌速度、介质离子强度、解吸温度和时间等实验条件 ;方法的线性范围为0.020~10μg/L ,检出限为0.008μg/L,相对标准偏差在6.8%~8.5 %之间 ,回收率在90%~94 %之间 ;分析海水样品发现赤潮海水中雪松醇的质量浓度是非赤潮海水的1~3倍 ,通过对海水中雪松醇质量浓度变化的监测 ,可能对赤潮的预报和防治提供依据 ;该法简便、快速、灵敏度高 。 展开更多
关键词 海水 SPME-GC-MS 测定 固相萃萃取 色谱-质谱法 雪松醇 赤潮 环境污染 环境监测
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A highly sensitive SPE-liquid/liquid extraction-RPLC analytical method for the determination of 6β-hydroxycortisol and cortisol in cancer patients' urine 被引量:3
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作者 Zhang Hong Fang Yu Li Ying Liang Aibin 《Journal of Medical Colleges of PLA(China)》 CAS 2010年第2期75-83,共9页
A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods: After SPE column purification and liquid-l... A highly sensitive SPE-liquid/liquid extraction RPLC method has been developed for the analysis of 6β-hydroxycortisol and cortisol in the urine of cancer patients. Methods: After SPE column purification and liquid-liquid extraction, the sample test solutions were analyzed with RPLC using a C18 analytical column. This improved analytical method has been validated for linearity, accuracy (recovery from urine), repeatability (within-day and between-day precision), specificity, sensitivity, and stability. This SPE-liquid/liquid extraction-RPLC is rapid, simple, accurate and reproducible. The technique is particularly useful for monitoring the CYP3A activity of cancer patients in clinical settings. The results are expressed as the ratio of 6β-hydroxycortisol to cortisol. Results: The CYP3A activity from a total of 153 samples was measured using this improved method. Considerable variation in the CYP3A activity of different cancer patients has been documented. Thus, personalized medical treatment based on the individual metabolic enzyme activity level is necessary. Conclusion: This new analytical method facilitates such individualized medical treatments. 展开更多
关键词 Solid phase extraction (SPE) Liquid/liquid extraction Reversed-phase high performance liquid chromatography (RPLC) CYP3A 6β-hydroxycortisol/cortisol Cancer
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Development of new solid phase extraction techniques in the last ten years 被引量:4
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作者 范惠霞 邓志鹏 +1 位作者 仲浩 姚庆强 《Journal of Chinese Pharmaceutical Sciences》 CAS CSCD 2013年第4期293-302,共10页
Solid phase extraction (SPE) is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of s... Solid phase extraction (SPE) is a widely used sample pretreatment method for separation, purification and enrichment, which has been established due to its significant advantages of time-saving, low consumption of solvent, high enrichment factor, high accuracy, etc. In recent years, a variety of new SPE methods such as molecularly imprinted solid phase extraction (MISPE), magnetic solid phase extraction (MSPE), solid phase micro-extraction (SPME), etc., which are superior to the conventional SPE, have been developed and been widely applied to food, drugs, and environmental monitoring. In this paper, the basic principles and methods of SPE and its new applications in different areas are reviewed. 展开更多
关键词 Solid phase extraction Molecularly imprinted solid phase extraction Magnetic solid phase extraction Solid phase micro-extraction
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A study revealing the key aroma compounds of steamed bread made by Chinese traditional sourdough 被引量:8
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作者 Guo-hua ZHANG Tao WU +4 位作者 Faizan A.SADIQ Huan-yi YANG Tong-jie LIU Hui RUAN Guo-qing HE 《Journal of Zhejiang University-Science B(Biomedicine & Biotechnology)》 SCIE CAS CSCD 2016年第10期787-797,共11页
Aroma of Chinese steamed bread(CSB) is one of the important parameters that determines the overall quality attributes and consumer acceptance. However, the aroma profile of CSB still remains poorly understood, mainl... Aroma of Chinese steamed bread(CSB) is one of the important parameters that determines the overall quality attributes and consumer acceptance. However, the aroma profile of CSB still remains poorly understood, mainly because of relying on only a single method for aroma extraction in previous studies. Therefore, the objective of this study was to determine the volatile aroma compounds of five different samples of CSB using three different aroma extraction methods, namely solid-phase microextraction(SPME), simultaneous distillation–extraction(SDE), and purge and trap(PT). All samples showed a unique aroma profile, which could be attributed to their unique microbial consortia.(E)-2-Nonenal and(E,E)-2,4-decadienal were the most prevalent aromatic compounds revealed by SDE, which have not been reported previously, while ethanol and acetic acid proved to be the most dominant compounds by both SPME and PT. Our approach of combining three different aroma extraction methods provided better insights into the aroma profile of CSB, which had remained largely unknown in previous studies. 展开更多
关键词 Steamed bread SOURDOUGH Simultaneous distillation–extraction(SDE) Solid-phase microextraction(SPME) Purge and trap(P&T)
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