沸石修饰聚丙烯酰胺复合材料富集——分光光度法测定日落黄色素

以沸石修饰聚丙烯酰胺复合材料作为固相萃取的吸附剂,与可见分光光度计联用检测软饮料中日落黄色素的含量。优化了固相萃取实验条件对萃取效率的影响,包括样品pH,样品流速,样品体积和洗脱液流速。在最优化的实验条件下,对5种软饮料中日落黄色素的含量进行了测定,日内、日间精密度分别为2.58%和4.63%;加标回收率范围为93.0%~98.7%。结果表明,本实验方法具有操作简单、灵敏度高、分析速度快等优点,适用于软饮料中日落黄色素的测定。     

高效液相色谱法测定烟草样品中的叶黄素和β-胡萝卜素

研究了用固相萃取和高效液相色谱法测定烟草样品中的叶黄素和β 胡萝卜素;烟草样品中的叶黄素和β 胡萝卜素用90%的丙酮震荡萃取,然后用WatersSep Park C18固相萃取小柱预分离和富集,以WaterNova Pak C18色谱柱为固定相,(1+1)甲醇异丙醇溶液 水梯度洗脱为流动相,二极管矩阵检测器检测测定。该方法标准回收率为96%～104%,RSD%为1.26%～2.43%;用于烟草中叶黄素和β 胡萝卜素的测定,结果满意。     

快速分离柱高效液相色谱法测定环境水样中多菌灵和噻菌灵的研究

研究并建立了用固相微萃取-快速分离柱高效液相色谱法测定环境水样中的多菌灵和噻菌灵的方法。样品中的多菌灵和噻菌灵用W aters Sep-pak C18反相固相萃取小柱预分离和富集,然后以ZORBAX Stab leBound(4.6 mm×50 mm,1.8μm)C18快速分离柱为固定相,甲醇-水(V(甲醇)/V(水)=1∶1)为流动相进行分离,流速为2.0 mL/m in;用二极管矩阵检测器检测,检测波长为286 nm,样品中的多菌灵和噻菌灵在2.0 m in内可达到基线分离。方法标准回收率为93%~104%,RSD为2.1%~3.2%。用新方法测定了环境水样中的多菌灵和噻菌灵,结果令人满意。     

SPE-快速分离柱HPLC法测定枸杞样品中的类胡萝卜素

研究了固相萃取(SPE)富集和预分离,快速分离柱高效液相色谱(HPLC)快速测定枸杞样品中类胡萝卜素的新方法;枸杞样品中的类胡萝卜素用W aters Sep-Pak C18固相萃取小柱预分离,然后以ZORBAX Stab leBound(4.6 mm×50 mm,1.8μm)快速分离柱为固定相,甲醇-四氢呋喃为流动相分离,V(甲醇)∶V(四氢呋喃)=80∶20,用二极管矩阵检测器检测,检测波长为450 nm,枸杞样品中的几种类胡萝卜素在5 m in内可达到基线分离,比常规方法节约时间75%左右。方法标准回收率为95%~103%,RSD为1.9%~2.6%。     

纳米氧化铝修饰硅胶复合材料富集-分光光度法测定柠檬黄色素

以纳米氧化铝修饰硅胶复合材料作为固相萃取吸附剂,与紫外-可见分光光度计联用检测饮料中柠檬黄色素的含量。讨论了固相萃取实验条件对萃取效率的影响,包括样品pH、样品体积、样品流速和洗脱液流速。在最优化的实验条件下,对6种饮料中柠檬黄色素的含量进行了测定,日内、日间精密度分别为2.36%和4.37%,加标回收率为94.5%~100.5%。结果表明,本实验方法具备操作简单、灵敏度高、分析速度快等优点,适用于饮料中柠檬黄色素的测定。     

固相萃取-高效液相色谱法同时测定水体中甲萘威和阿特拉津

建立了一种固相萃取-高效液相色谱法同时测定水中甲萘威和阿特拉津浓度的方法。水样用C18固相柱萃取,以甲醇溶剂洗脱定容后,通过条件优化,确定检测波长为222 nm,流动相比例为6:4(甲醇:水),流速为0.8 mL/min,柱温度为40℃。在该条件下,甲萘威和阿特拉津在0.05～5 mg/L范围内相关系数分别为0.9999和0.9998,萃取水样100 mL时检出限分别为0.00002 mg/L和0.00005 mg/L,测定标准样品的准确度分别为97.4%和97.5%,实际水样加标回收率分别为75.4%～89.7%和76.1%～91.7%,测定结果的相对标准偏差分别为5.10%～8.85%和3.26%～7.44%。该方法简单便捷、灵敏准确,适用于同时测定水体中的甲萘威和阿特拉津。     

国内气相色谱-质谱联用分析技术在氨基甲酸乙酯检测中的应用

气相色谱-质谱法是测定发酵食品和酒精饮料中氨基甲酸乙酯非常重要的方法,相关的报道也非常多。为了适应不同基质样品的分析,需采用不同的样品前处理方法。文章介绍了液/液萃取(LLE)、固相萃取(SPE)、固相微萃取(SPME)等9种样品前处理方法结合气相色谱/气质联用技术在检测氨基甲酸乙酯中的应用。     

高效液相色谱测定水中微囊藻毒素

应用高效液相色谱法测定水中微囊藻毒素的含量.水样经C18柱固相萃取后进行HPLC分析.通过优化固相萃取方法,采用Symmentry C18色谱柱,以甲醇：水（含0.05%三氟乙酸）=60：40（V/V）溶液为流动相,紫外238nm检测.对两种常见微囊藻毒素MC-RR、MC-LR的检测限为0.02～0.05μg/L.实验表明该法可有效检测水样中的痕量微囊藻毒素.     

聚合物整体柱在固相萃取领域的应用

由于医药、生物、环境、食品等样品组成复杂,待测物含量低,常常需要在分析测定之前对样品进行前处理以达到净化富集的目的。基于聚合物整体柱制备简单、生物兼容性良好、比表面积大、传质速度快等优点,近年来受到广泛关注。本文主要介绍了聚合物整体柱的分类,将其作为固相萃取吸附剂在食品安全,生物富集,环境评价,医药卫生等方面的应用,同时展望了聚合物整体柱在固相萃取领域的发展趋势。     

三聚氰胺分子印迹固相萃取小柱的研制及其应用

用本体聚合法制备三聚氰胺分子印迹聚合物,通过静态平衡吸附实验及固相萃取实验表征其固相萃取性能,结合HPLC法对实际奶粉样品中的三聚氰胺进行测定.三聚氰胺模板聚合物的吸附能力强于空白聚合物;固相萃取柱对三聚氰胺标准溶液(0.3 mmoL/L)一次性萃取率达97.01%,奶粉样品中三聚氰胺测定的平均回收率为101.2%.印...     

A novel acrylamide modified primary-secondary amine analogue as impurities remover for determination of carbendazim and dimethyl phthalate in apples

A novel acrylamide modified Primary-Secondary Amine (PSA) analogue (acrylamide/3-aminopropyltriethoxysilane/ silica) was prepared and used as impurities remover for pesticide residues (carbendazim and dimethyl phthalate) in apples by QuEChERS combined with pipette-tip micro solid-phase extraction method. The properties of acrylamide/3-aminopropyltriethoxysilane/silica were characterized by scanning electron microscopy and Fourier transform infrared spectroscopy. Under the optimized conditions, factors such as amount and type of adsorbents were investigated. The limit of detection and limit of quantity of the method were 0.012 μg/mL and 0.04 μg/mL for carbendazim, 0.023 μg/mL and 0.08 μg/mL for dimethyl phthalate, respectively. The recoveries of proposed method at three spiked levels analysis were 84.9–90.0% for carbendazim and 84.1–88.2% for dimethyl phthalate, respectively, with the relative standard deviation less than 2.9%. The acrylamide/3-aminopropyltriethoxysilane/silica as potential adsorbent showed strong ability for removing the matrix, and it achieved great ability to retain the targets. It will provide a new material choice for detecting pesticide residues in apple samples.     

心血管中药方剂暖心方微波提取

因煎煮法等传统萃取方法不适用于提取热稳定性低的成分、萃取率不高，且目前研究主要集中于对单一药材的提取，故本研究使用微波提取技术提取中药复方（暖心方）中的有效成分；采用HPLC技术对提取液中有效成分含量进行分析；采用单因素实验法探究微波功率、萃取时间、提取次数三个因素对提取工艺的影响；此外，通过SEM对细胞破壁情况分析，了解其微波提取机理。实验结果显示，微波提取有效成分的最佳提取条件为：微波功率1200 W、萃取时间40 min、提取次数1次。与传统加热萃取法相比，微波辅助萃取技术能明显地缩短萃取时间，实现了节能高效。微波辐射因能深入并作用于中药材内部，使细胞壁破损，更好地将中药材中的有效成分析出。     

Quality assurance of Chinese herbal medicines: Procedure for multiple‐herb extraction

A quality assurance (QA) procedure for multiple‐herb extraction, which takes into account the existence of common chemical markers and multiple‐herb‐extraction effects, has been developed for producing Chinese herbal medicines (CHMs) of consistent quality. The experimental method for determining related correlation function of the multiple‐herb‐extraction effect was designed. A systematic solution strategy was also developed to appropriately decompose the multiple‐herb extraction system into several subsystems for obtaining solution(s) and determining the overall behavior of the system. An example of QA of Danshen–Gegen (DG) decoction was used to demonstrate the QA procedure. An H9c2 cell assay was used to test the efficacy of consistent quality DG decoctions prepared by different herb combinations with different material costs of herbs. It was observed that a multiple‐herb‐extraction effect was present in the aqueous extraction of Danshensu and this effect was depended on the extraction solvent. The possible mechanism of this multiple‐herb‐extraction effect in the aqueous DG extraction was speculated to be the change of initial pH value of the aqueous extraction solvent by an unknown component from Gegen. The experimental chemical marker concentrations fell within ±10% of the specified chemical marker compositions by using the amount of herb from each herb class as predicted by the QA model. Furthermore, an H9c2 cell assay was used to test the efficacy of three consistent quality DG extracts, which were produced by different herb combinations with different material costs of herbs. The results showed that the three DG extracts provided consistent biological efficacy against menadione‐induced toxicity. This study extended a recently developed QA procedure of single‐herb extraction to multiple‐herb extraction. It provides a solution of QA in extraction, which is one of the most important unresolved problems in the modernization of traditional Chinese medicines. With this modified model and the companion experiments, the amount of herbs needed from different quality classes to produce a multiple‐herb formula CHM product decoction with consistent quality can be exactly determined. © 2014 American Institute of Chemical Engineers AIChE J 60: 4014–4026, 2014     

分子印迹固相萃取法提取花生壳中木犀草素

采用分子印迹技术,以木犀草素为模板分子、丙烯酰胺为功能单体、EGDMA为交联剂,合成了木犀草素印迹聚合物。将该印迹聚合物用于固相萃取,分离提取花生壳中的木犀草素。结果表明,该印迹聚合物对木犀草素具有较高的吸附性能和选择性,用印迹柱萃取得到的木犀草素纯度高出硅胶柱分离近20个百分点,达到96.2%。且MIPs-SPE柱与普通的硅胶柱相比,经过洗脱再生后可以反复使用多次。     

Preparation and adsorption selectivity of deltamethrin molecularly imprinted polymers by two-step seed swelling method

Deltamethrin (DM) is one of the most efficient pyrethroid insecticides, which is widely applied to the control of insect pests in tea. In this work, efficient molecularly imprinted polymers (MIPs) were synthesized using DM as the template and acrylamide as the functional monomer, in conjunction with two-step seed swelling polymerization. Scanning electron microscopy, Fourier transform infrared spectroscopy, and Brunauer–Emmett–Teller surface area analysis confirmed the staggered pore structure and the presence of binding site in DM MIPs. The adsorption properties of the DM MIPs were also investigated based on assessing equilibrium adsorption as well as kinetic modeling and solid-phase extraction. Isothermal equilibrium adsorption experiments show that the adsorption behavior is consistent with the Freundlich and Halsey models, indicating heterogeneous multilayer specific adsorption. Fitting of the kinetic data demonstrates that chemical adsorption could be the rate-limiting step in DM extraction, which is consistent with a pseudo-second-order kinetic model. Using the imprinted polymers as solid-phase extraction filler, the DM recoveries from various teas were greater than 80% and exceeded those of the structural analogs cypermethrin, lambda-cyhalothrin, and bifenthrin. These results confirm that the MIPs exhibit specific adsorption of this analyte. © 2018 Wiley Periodicals, Inc. J. Appl. Polym. Sci. 2019 , 136, 47415.     

鱼腥草中槲皮素的提取及含量测定

采用超声波法提取鱼腥草中的槲皮素,通过单因素实验和正交实验确定最佳提取条件为：提取温度80℃、提取时间45 min、乙醇体积分数80％.在最佳提取条件下,提取不同产地鱼腥草中不同部位槲皮素并进行含量测定及对比.结果表明：不同产地鱼腥草中槲皮素的含量差异较大,且鱼腥草叶中槲皮素的含量明显较高,是根茎中的6～17倍.高效液相色谱法精密度高、重现性好,适用于中草药中槲皮素含量的测定.     

三羟基丙烷交联聚氨酯/有机硅固相微萃取涂层的研制和应用

通过三羟基丙烷交联聚氨酯/有机硅合成了有机硅/聚氨酯共聚物,将其涂渍于纤维丝上制成了固相微萃取(SPME)探头并安装于SPME装置上,与气相色谱联用测定了水中氯苯等芳香化合物。考察了该共聚物制成的萃取头热稳定性及使用寿命、影响萃取效率的因素。结果表明:有机硅/聚氨酯共聚物涂层具有使用寿命长(100次以上)、成本低、耐高温(270℃)等特点,对样品中氯苯等芳香化合物的萃取效果优于其它探头。本方法检出限低(0.05～0.5μg/L),重现性好(RSD4.8%～5.9%)。     

氧化铝干柱固相萃取结合紫外导数光谱法快速测定全血安定

建立一种简便的血中安定的测定方法.采用氧化铝干柱层析固相萃取血中安定,紫外二阶导数光谱法测定萃取液中安定药物浓度.对于血液中安定含量在mg/L级时,pH=7条件下的萃取回收率〉89%,RSD〈10%.本方法简便易行、材料价廉,对于含安定mg/L级的血样,测定结果准确可靠,批量测试更省时间.     

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。     

快速GC-MS法分析炸薯片中丙烯酰胺

开发了一种用于分析炸薯片中丙烯酰胺的快速GC-MS方法,经过提取、脱脂、净化、溴化衍生、萃取等过程,最后转化成2-溴丙烯酰胺进行GC-MS分析.研究表明,脱脂和净化过程中丙烯酰胺的损失率分别为2.57%和0·66%,测量问的相对标准偏差小于10%,加样回收率高达91.02%,检测线性范围为50～50000μg·kg-1,检测限、定量限分别为5μg·kg-1和20μg·kg-1.具有低成本、快速、稳定的优点,适用于炸薯片中丙烯酰胺的定量检测.