利用分散液-液微萃取和反相高效液相色谱-荧光检测器测定硒蛋白多糖中硒含量

本试验介绍了一种利用分散液-液微萃取前处理并将一种新型反相色谱柱应用于高效液相色谱-荧光检测器(HPLC-FLD)测定硒蛋白多糖中硒含量的方法。该方法以2,3-二氨基萘(DAN)为螯合剂,400μL乙腈为分散剂,120μL氯苯为萃取剂,硒(Ⅳ)与2,3-二氨基萘的螯合物(Se-DAN螯合物)经乙腈稀释后进行高效液相色谱分析。采用PFP色谱柱分离,乙腈为流动相,用荧光检测器在激发波长为376 nm、发射波长为520 nm条件下测定荧光强度,外标法定量。结果显示:该方法成功地用于测定硒蛋白多糖中硒含量,硒的检出限为2.5μg/L,线性范围为5.0~250.0μg/L。采用该方法测定的硒蛋白多糖中硒含量为1337.0μg/g,与荧光分光光度法(国标法)测定结果高度一致;并且,该方法也适用于酵母硒中硒含量的测定。本试验成功建立了检测硒蛋白多糖中硒含量的方法,该方法具有操作简便、易普及、试剂消耗少、分离度好、回收率高和适用性强等特点。     

固相萃取——高效液相色谱法分离红花中的黄酮类物质

目的 研究红花中的黄酮类物质。方法 乙醇浸泡提取，固相萃取分离，液相色谱法进行纯度检测，结果 采用的红花中有两种黄酮类物质。结论 洗脱液V（H2O）：V（C4H5OH）=3：7，能很好的分离红花中的两种黄酮类物质。     

Chemical Synthesis and Structure-Activity Relationship Study Yield Desotamide a Analogues with Improved Antibacterial Activity

Desotamides A, a cyclohexapeptide produced by the deep-sea-derived Streptomyces scopuliridis SCSIO ZJ46, displays notable antibacterial activities against strains of Streptococcus pnuemoniae, Staphylococcus aureus, and methicillin-resistant Staphylococcus epidermidis (MRSE). In this study, to further explore its antibacterial potential and reveal the antibacterial structure-activity relationship of desotamides, 13 cyclopeptides including 10 new synthetic desotamide A analogues and wollamides B/B1/B2 were synthesized and evaluated for their antibacterial activities against a panel of Gram-positive and -negative pathogens. The bioactivity data reveal that residues at position II and VI greatly impact antibacterial activity. The most potent antibacterial analogues are desotamide A4 (13) and A6 (15) where l-allo-Ile at position II was substituted with l-Ile and Gly at position VI was simultaneously replaced by d-Lys or d-Arg; desotamides A4 (13) and A6 (15) showed a 2–4-fold increase of antibacterial activities against a series of Gram-positive pathogens including the prevalent clinical drug-resistant pathogen methicillin-resistant Staphylococcus aureus (MRSA) with MIC values of 8–32 μg/mL compared to the original desotamide A. The enhanced antibacterial activity, broad antibacterial spectrum of desotamides A4 and A6 highlighted their potential as new antibiotic leads for further development.     

结香鲜花香气化学成分的研究

采用固相微萃取(SPME)吸附采集结香(Edgeworthia chrysantha Lindl.)鲜花的香气成分，用色谱-质谱联用分析鉴定，并用GC-MS总离子流色谱峰的峰面积进行归一化定量分析结香鲜花的香气成分，鉴定出γ-萜品烯56．41％、乙酸苄酯10．77％、β-苯乙基乙酸酯9．58％、3，7-二甲基-2，6-辛二烯-1-醇乙酯5．61％、水杨酸甲酯3．91％、苯甲酸甲酯2．85％、反式罗勒烯1．80％、苯甲醛1．75％和3-甲基-3-癸烯-2-酮1．40％等30种化合物。固相微萃取-气相色谱-质谱法是一种可用于鲜花香气成分分析的简单可行的分析方法。     

竹醋液烟熏气化学成分的研究

采用固相微萃取(SPME)吸附采集竹醋液烟熏气的成分,用气相色谱—质谱联用分析鉴定,并用GC/MS总离子流色谱峰的峰面积进行归一化定量分析竹醋液烟熏气成分,鉴定出愈创木酚11.36%、苯酚10.6%、4-乙基苯酚8.23%、2-甲氧基-4-甲基苯酚7.08%、4-乙基-2-甲氧基苯酚6.6%、2-乙基苯酚5.65%、糠醛5.51%、5-甲基糖醛1.47%、乙酸1.42%、3-甲基-1-戊烯-3-醇1.42%、2,3-二甲基甲苯1.35%、2-糠酸甲酯1.35%、苯甲酸甲酯1.11%、2-甲基-2-环戊烯-1-酮1.44%、2,3-二甲基-2-环戊烯-1-酮1.31%、2-环戊烯-1-酮1.02%等74种化合物。竹醋液烟熏气的所有成分是竹醋液化学成分的特征性组成部分。     

鹿角杜鹃开花过程中挥发性成分的变化

利用顶空固相微萃取-气相色谱质谱法,对鹿角杜鹃Rhododendron latoucheae花朵在花蕾期、半开放期、盛开期及凋落期4个开花期的挥发性成分进行了定性和相对定量分析,研究了鹿角杜鹃花香成分的种类和变化情况.结果表明,在鹿角杜鹃花朵开放的4个时期中共检测出37种挥发性成分,这些挥发性成分种类在开花过程中呈升高...     

固相萃取-高效液相色谱法测定生姜中涕灭威及其代谢物

建立了生姜中涕灭威、涕灭威砜和涕灭威亚砜残留量检测的固相萃取—高效液相色谱分析方法。样本采用乙腈提取,经C18固相萃取柱净化,浓缩定容后用HPLC-FLD检测分析,外标法定量。结果表明:该方法在0.02~8.0 mg/L标准曲线线性良好,相关系数均达到0.999以上,样本添加水平为2.0×10-2、4.0×10-2mg/kg时,回收率为80.25%~102.85%,相对标准偏差为3.64%~8.67%,方法检出限均低于2.5×10-3mg/kg。该方法具有准确度高及净化效果好等特点,能很好地满足实际样本残留分析要求。     

金银花和红银花挥发性成分的顶空固相微萃取#br# 气质联用检测与比较

 采用顶空固相微萃取气质联用（SPME–GC–MS）的方法检测红银花与金银花新鲜花蕾和 干花蕾的挥发性成分。4 种花蕾样品共鉴定出67 种挥发性物质,其中新鲜红银花与金银花分别检测出48 种和46 种,经烘干处理的干红银花与金银花分别检测出34 种和37 种。[3.2.1.0（1,5）]三环辛烷、β– 芳樟醇、5–甲基–2–己醇和以及十六烷是4 种样品共有的成分。其中红银花挥发性成分主要以烃类、 醇酮类为主,β–芳樟醇含量显著高于金银花;样品在由新鲜到烘干这一过程中,烃类和酯类挥发性物质 含量降低,醛类和醇酮类挥发性物质显著增加。     

Interference elimination of PCB and its ramification in determining trace PBBs/PBDEs by GC/MS

The normal method to determine the trace brominated flame retardants such as polybrominated biphenyls (PBBs) and polybrominated diphenylethers (PBDEs) contained in the electronic and electrical products is gas chromatography/mass spectrometry (GC/MS). However, the method is based on the determinations of the persistent organic pollutants (POPs) such as polychlorinated biphenyls (PCBs), and polychlorinated naphthalene (PCNs) etc. The interferences of those compounds are inevitable. Therefore, in order to overcome this problem, two methods e.g. 1) The combination use of gas chromatography negative ion chemical ionization mass spectrometry (GC-NICI-MS) and gas chromatography-electron impact-mass spectrometry (GC-EI-MS) is employed, 2) a matrix solid-phase dispersion (MSPD) method with YMC ODS-C18 as carrier is developed. The result show that, by the former method, the brominated isomers or ramifications are distinguished remarkably from other halogen compounds because that anion fragment retention peaks of ［Br］-, ［HBr2］- and molecule chain fragment retention peaks of ［M+2］+,［M+4］+,［M+6］+,［M+8］+ are observed simultaneously, and thus the selectivity to determine bromine-containing retardant flames is greatly improved. Using the latter method, the gas chromatographic peaks of multiple polychlorinated biphenyls and polybrominated diphenylethers can be efficiently separated. Thus provides a project to solve interferences of POPs in brominated flame retardants’ determinations. The standard addition experimental results of 10 kinds of BDEs/PCBs belonging to 8 sorts of electronic and electrical equipment show this method has a high precision and reliability due to 60%～98% recovery and <9.5% relative error, which meet the needs regulated by the IEC Commission. It provides a technical support for electronic and eletrical industries in China to further comply with RoHS directive.     

紫丁香鲜花香气化学成分的研究

采用固相微萃取吸附采集紫丁香Syringa oblata鲜花的香气成分,用色谱/质谱联用分析鉴定,并用GC/MS总离子流色谱峰的峰面积归一化法对紫丁香鲜花的挥发性成分进行定量分析。结果鉴定出大香叶烯-D(22.37%)、β-波旁烯(15.97%)、苯甲醛(11.03%)、β-石竹烯(7.56%)、β-古芹烯(3.43%)、芳樟醇(3.18%)、丁香醛B(2.99%)、α-胡椒烯(2.70%)、β-苯乙醇(2.39%)、苯乙醛(1.99%)、苯甲醇(1.89%)、丁香醇B(1.87%)、α-愈创木烯(1.49%)、丁香醛A(1.46%)、α-蒎烯(1.39%)、丁香醇A(1.03%)、α-草烯(1.03%)等48种化合物。其中所含的4个丁香醇异构体和2个丁香醛异构体是紫丁香鲜花的特征香气成分。固相微萃取-气相色谱/质谱法是一种可用于鲜花挥发性香气成分分析的简单可行的分析方法。图1表1参10