气相色谱法同时测定茶叶中10种有机磷农药残留

目的建立用气相色谱法同时测定茶叶中10种有机磷农药残留的方法。方法采用乙腈做萃取溶剂超声波提取,经CARB/NH2固相萃取小柱净化,用气相色谱法FPD检测器检测茶叶中10种有机磷农药。结果在0.05~1.0 mg/kg浓度范围内具有良好的线性关系,相关系数为0.999 63~0.999 86;在有机磷农药添加浓度为0.02~1.0 mg/kg,回收率80.0%~102.0%,相对标准偏差1.8%~5.8%,最低检出限(LOD,S/N=3)为0.002~0.013 mg/kg。结论建立的气相色谱法是一种操作简单、分离效果好、回收率高、方便快速的检测方法。     

香水鱼调料中多种有机磷农药残留的测定

建立凝胶渗透色谱净化-气相色谱法测定香水鱼调料中的14种有机磷农药残留的方法。样品中的有机磷农药用乙腈提取,凝胶渗透色谱净化,经毛细管柱(DB-1701P,30 m×0.25 mm×0.25μm)分离,气相色谱-火焰光度检测器(FPD)检测。方法检出限为0.002 6 mg/kg～0.033 mg/kg;相对标准偏差(n=5)为1.0%～12.6%;14种有机磷农药平均回收率在75.82%～123.50%,该方法能满足香水鱼调料中有机磷农残测定的要求。     

加速溶剂提取-凝胶渗透色谱净化-气相色谱测定咸鱼中的敌敌畏

建立咸鱼中敌敌畏残留的气相色谱分析方法。采用加速溶剂萃取(ASE)提取咸鱼样品中的敌敌畏,经凝胶渗透色谱(GPC)净化,浓缩定容后用GC-FPD 检测分析,外标法定量。样品添加水平为2.5 × 10-2mg/kg 和10.0 ×10-2mg/kg 时,敌敌畏的回收率在74.4%～96.8% 之间,方法检出限为5.0 × 10-4mg/kg。本方法准确、自动化程度高、净化效果好,满足残留分析要求。     

菜籽油中5种高毒农药GPC-GC-MS/MS检测方法

建立凝胶渗透色谱―气相色谱―串联质谱法测定菜籽油中5种高毒农药的检测方法。样品经乙酸乙酯―环己烷(体积比1∶1)溶解,凝胶渗透色谱(GPC)净化,利用GC–MS/MS检测,外标法定量。方法检测限为0.2~1.9μg/kg,在0.05、0.1、0.5 mg/kg三个质量分数水平进行了添加回收实验,样品回收率为75.2%~95.7%,RSD为2.0%~6.1%。该方法具有操作简单,快速,净化效果好,精密度高,重现性好等优点,可应用于菜籽油中的5种高毒农药残留量的检测。     

凝胶渗透色谱-气相色谱-质谱法测定食用植物油中120种农药残留量

本实验建立了气相色谱-质谱法(GC-MS),同时测定植物油中120种农药的多残留分析方法。样品用正己烷溶解,乙腈萃取,凝胶渗透色谱(GPC)净化,GC-MS测定,外标法定量。方法定量下限检出限(S/N≥10)为0.005~0.100 mg/kg,在加标水平为0.05 mg/kg时,方法回收率为67.1%~120%,相对标准偏差RSD在20%以内。     

凝胶渗透色谱-高效液相色谱串联质谱法测定咸鱼中7种有机磷农药

目的建立咸鱼中丙溴磷、毒死蜱、马拉硫磷、亚胺硫磷、三唑磷、敌百虫和乐果等7种有机磷农药的凝胶渗透色谱-高效液相色谱串联质谱测定法。方法咸鱼样品经环己烷.乙酸乙酯(l:l,v:v)提取后,经凝胶渗透色谱仪净化,再使用Extend-C_(18)色谱柱分离,采用电喷雾离子化源,以多反应监测(MRM)方式分析,正离子化模式进行检测。结果 7种有机磷农药在2.5~100μg/kg线性范围内的相关系数良好,其检出限在0.05~0.20μg/kg之间。该方法加标回收率为70.9%~116.6%,相对标准偏差为2.7%~13.8%(n=6)。结论本方法具有提取效率高,净化效果好,准确灵敏和快速等优点,适用于咸鱼中有机磷农药残留检测,符合实际工作需要。     

凝胶渗透色谱净化结合气相色谱-三重四极杆质谱法测定植物油中多农药残留量

建立了凝胶渗透色谱法结合气相色谱-三重四极杆质谱测定植物油中多种类型农药残留的方法(有机磷农药、有机氯农药、拟除虫菊酯农药、氨基甲酸酯农药、三唑类杀菌剂、植物生长调节剂等)。样品使用乙酸乙酯-环己烷(1∶1,V/V)溶解后,经全自动凝胶渗透色谱仪净化,色谱柱流速为5 m L/min,收集时间为7~20 min,然后进行在线自动真空浓缩,正己烷溶剂将样品定容到1.0 m L,使用气相色谱-三重四极杆质谱仪的选择反应监测模式进行定性和定量分析。在相应线性范围内,所有化合物线性关系良好,线性相关系数R2在0.990 0~0.998 5之间。在0.05~0.40 mg/kg添加水平时,平均回收率为60.5%~118.0%,相对标准偏差(RSDs,n=6)为1.3%~14.5%,检出限在0.002~0.01 mg/kg之间,满足国内外对植物油中农药最大残留限量的标准要求。     

固相萃取-高效液相色谱荧光法测定水果中1-萘乙酸残留量

建立了固相萃取-高效液相色谱荧光法测定水果中1-萘乙酸(NAA)残留量的方法。样品经乙腈提取,氨基固相萃取小柱净化,用高效液相色谱荧光检测器测定。经过验证,方法定量限为0.002 mg/kg,当水果中添加NAA水平为0.004、0.04、0.4 mg/kg时,回收率为82.1%~114.1%之间,相对标准偏差(RSD)为0.6%~10.5%。该方法准确度好、灵敏度高,适合水果中NAA残留量的测定。     

加速溶剂萃取/凝胶渗透色谱净化/气相色谱-三重四极杆质谱测定水产品中的持久性有机污染物

建立了一种加速溶剂萃取/凝胶渗透色谱净化/气相色谱三重四极杆质谱同时检测水产品中46种典型持久性有机污染物的方法。水产样品经-105℃、100 mbar条件下的冷冻干燥处理后,加入硅藻土混合碾磨均匀后,经加速溶剂萃取、凝胶渗透色谱净化,使用萘-d、芴-d、蒽-d、■-d作为内标,采用气相色谱三重四极杆质谱的多反应监测模式对水产品中的16种多环芳烃、30种有机氯农药进行定性定量分析。在100℃、1500 psi条件下以二氯甲烷:己烷(1:1,V/V)对46种有机污染物进行萃取,收集凝胶渗透色谱中7.5~16 min馏出液,浓缩定容上机分析。46种持久性有机污染物分离效果良好,相关系数R^2均在0.99以上,低(10μg/kg)、中(50μg/kg)、高(100μg/kg)3个水平的加标回收率均在81.0%~121.0%之间,相对标准偏差(RSD,n=6)在4.1%~11.0%之间,方法检出限为0.0185μg/kg^0.7377μg/kg(干重)。该方法采用加速溶剂萃取仪和凝胶渗透色谱仪进行前处理,可实现前处理无人值守,大大提升检验效率,且方法稳定性好,灵敏度和回收率高,是分析水产品中痕量持久性有机污染物的较好方法。     

气相色谱-质谱法检测干辣椒中常用有机磷和拟除虫菊酯类农药的残留

目的建立凝胶色谱技术(GPC)净化和气相色谱质谱法同时测定干辣椒中常用有机磷和拟除虫菊酯类农药的测定方法。方法样品采用乙腈-水提取,经凝胶色谱仪净化去除大分子色素及杂质,再经过石墨化炭黑-氨基SPE柱净化,以气相色谱-质谱联用仪(EI源)检测,内标法定量。结果在添加水平为0.05~0.5 mg/kg下的平均回收率为71.6%~116.4%,相对标准偏差在2.3%~10.8%之间,样品最低检出限为0.01~0.05 mg/kg。结论此方法净化效果显著,测定结果准确,实验周期短,基本实现全自动化,节省大量时间与试剂,适用于大批量辣椒的农药残留检测。     

Green Extraction Methods for Polyphenols from Plant Matrices and Their Byproducts: A Review

Polyphenols as phytochemicals have gained significant importance owing to several associated health benefits with regard to lifestyle diseases and oxidative stress. To date, the development of a single standard method for efficient and rapid extraction of polyphenols from plant matrices has remained a challenge due to the inherent limitations of various conventional extraction methods. The exploitation of polyphenols as bioactive compounds at various commercial levels has motivated scientists to explore more eco‐friendly, efficient, and cost‐effective extraction techniques, based on a green extraction approach. The current review aims to provide updated technical information about extraction mechanisms, their advantages and disadvantages, and factors affecting efficiencies, and also presents a comparative overview of applications of the following modern green extraction techniques—supercritical fluid extraction, ultrasound‐assisted extraction, microwave‐assisted extraction, pressurized liquid extraction, and pressurized hot water extraction—as alternatives to conventional extraction methods for polyphenol extraction. These techniques are proving to be promising for the extraction of thermolabile phenolic compounds due to their advantages over conventional, time‐consuming, and laborious extraction techniques, such as reduced solvent use and time and energy consumption and higher recovery rates with lower operational costs. The growing interest in plant‐derived polyphenols prompts continual search for green and economically feasible modern extraction techniques. Modern green extraction techniques represent promising approaches by virtue of overcoming current limitations to the exploitation of polyphenols as bioactive compounds to explore their wide‐reaching applications on an industrial scale and in emerging global markets. Future research is needed in order to remove the technical barriers to scale‐up the processes for industrial needs by increasing our understanding and improving the design of modern extraction operations.     

Combination of emerging technologies for the extraction of bioactive compounds

Abstract

With the growing consumer demands for greener alternatives that do not involve toxic chemicals as well as the industry concerns of sustainable, nontoxic routes of extraction, the applications of novel extraction technologies in the food industry have been widely studied. This review discussed the novel extraction technologies including their mechanisms, protocols, influencing factors, advantages and drawbacks, as well as a comprehensive summary of the combination of the novel extraction technologies for phyto-bioactive compounds. Novel extraction methods, including ultrasound-assisted extraction (UAE), microwave-assisted extraction (MAE) and enzyme-assisted extraction (EAE), are considered as clean, green and efficient alternative to conventional extraction technologies. Their combinations, ultrasound-assisted enzymatic extraction (UAEE), microwave-assisted enzymatic extraction (MAEE) and ultrasonic microwave-assisted extraction (UMAE), can exhibit higher potential extraction ability. However, some of them need specific equipment. The food industry in the extraction sector should choose a proper extraction method which has a balance between product quality, process efficiency, production costs and environmentally friendly processes. The current review presented comprehensive references for future research on the novel extraction of phyto-bioactive compounds extraction.

1. Highlights

2. Novel clean, green and efficient alternative to conventional extraction technologies are discussed.

3. Combination of the novel extraction technologies for synergistic effects.

4. Minimal degradation and enhanced extraction yields.

5. Extraction mechanisms, advantages and drawbacks associated with novel extraction technologies.

     

炒芝麻的挥发性成分分析

采用四种前处理方法(直接溶剂萃取、固相微萃取、同时蒸馏萃取、顶空蒸馏萃取)提取炒芝麻挥发性成分,经GC-MS分析鉴定并根据鉴定结果调配炒芝麻香精。对香精进行评价得到得到以下结论:直接溶剂萃取法适合处理含油量较小的样品,同时蒸馏萃取法适合处理对热不敏感的样品,顶空蒸馏萃取法适合处理对热敏感的样品。     

同时蒸馏萃取和固相微萃取对双孢蘑菇风味物质的提取分析

采用同时蒸馏萃取法和固相微萃取法对双孢蘑菇的挥发性风味物质进行提取,并通过气相色谱-质谱联用分析及鉴定。采用同时蒸馏萃取法鉴定出36种化合物,采用固相微萃取法鉴定出34种风味化合物,2种方法分析出蘑菇的特征风味物质为1-辛烯-3-醇、1-辛烯-3-酮、2-辛烯-1-醇、2,6-二甲基吡嗪、2-戊基呋喃、甲基吡嗪、1-辛醇等,均以1-辛烯-3-醇含量最高。2种提取方式相互补充相互验证。     

多壁碳纳米管分散固相萃取净化在测定水产品中3 种微囊藻毒素的应用及与固相萃取法的比较

建立多壁碳纳米管净化-超高效液相色谱-串联质谱法对水产品中3?种微囊藻毒素残留量的测定方法。水产品用80%甲醇溶液提取,经多壁碳纳米管净化后,采用电喷雾正离子多反应监测模式进行分析。对不同性质碳纳米管进行考察,并对净化条件进行优化。将优化后的分散固相萃取条件与采用HLB柱固相萃取的净化方式进行比较,两者在1～50?μg/L范围内呈现良好的线性,线性相关系数均大于0.99,3?种微囊藻毒素的检出限为0.1～0.2?μg/kg。在不同浓度水平下进行加标实验,平均回收率在88.7%～95.5%之间,相对标准偏差不大于4.2%。该方法适用于水产品中微囊藻毒素的痕量检测。     

超声辅助提取技术在天然产物提取中的应用

简述超声辅助提取技术提高活性成分提取率的作用及原理,对超声辅助提取技术在天然产物有效成分(生物碱、黄酮、蒽醌、皂甙、植物油)提取方面,以及在农残分析样品提取方面的应用研究成果进行概述,并指出当前研究中存在的问题和今后的研究方向。     

茶饮料浸提工艺的微波辅助萃取(MAE)应用研究

浸提工艺是茶饮料生产过程一个关键生产工艺。本文比较了传统热水浸提工艺和微波辅助萃取工艺之间的最优工艺参数，并利用高效液相色谱分析方法研究了微波萃取对茶多酚浸出得率和单体组成的影响，表明微波萃取技术（Microwave-assisted extraction，MAE）可应用在茶饮料生产中，而且比传统热水浸提工艺省时节能。结果表明：传统热水浸提工艺的最优浸提温度90℃、时间43min、液固比20：1，茶多酚的得率为19．76％；微波辅助萃取工艺的最优浸提功率360W、时间3、5min、液固比25：1，茶多酚的得率为20．63％。微波短时处理茶叶不会对茶多酚的结构和单体组戍产生破坏性影响。     

羊栖菜粗多糖的提取工艺

通过单因子试验 ,将响应面分析法 (RSA)应用于羊栖菜粗多糖提取工艺的研究 ,采用合理的试验设计对提取工艺进行全面研究 ,依据回归分析确定工艺条件的影响因子 ,从而求得最佳水浸提工艺条件 :提取温度 85℃、浸提时间 2 6h、水料比 2 8∶1 ,醇析浓度 80 %,浸提 1次时 ,羊栖菜粗多糖的提取率为 1 1 1 2 %。