阿斯美胶囊中四种组分的高效液相色谱分析

建立了反相高效液相色谱法测定阿斯美胶囊中氨茶碱、盐酸甲氧非那明、马来酸氯苯那敏及那可汀四种组分的含量。色谱柱为ＳｐｈｅｒｉｓｏｒｂＣ８，５μｍ，２００ｃｍ×４０ｍｍＩＤ，流动相为体积分数０５％的三乙胺溶液（磷酸调节ｐＨ５５）＋乙腈＋甲醇（５５０＋３６８＋８２），检测波长为２６４ｎｍ，线性范围分别为：氨茶碱３１２５～２５０ｍｇ／Ｌ，γ＝０９９９６，盐酸甲氧非那明１５６２５～１２５０ｍｇ／Ｌ，γ＝１００００，马来酸氯苯那敏２５～２００ｍｇ／Ｌ，γ＝０９９９９，那可汀８７５～７００ｍｇ／Ｌ，γ＝０９９９９；回收率（ｎ＝３）分别为１０１２％，１００８％，９９９％，９９５％；精密度：日内平均ＲＳＤ（ｎ＝６）分别为０７％，０４％，０４％，０６％；日间平均ＲＳＤ（ｎ＝３）分别为１０％，１０％，１１％，１２％。     

高效液相色谱法测定灭尔痛片的组分含量

采用高效液相色谱法同时测定灭尔痛片中对乙酰氨基酚、异丙基安替比林、及咖啡因３种成分的含量。色谱条件为：ＯＤＳ柱，甲醇＋水（６０＋４０）为流动相，检测波长为２５４ｎｍ。方法线性范围分别为：２４～１２０ｍｇ／Ｌ（ｒ＝０９９７６）；１２～６０ｍｇ／Ｌ（ｒ＝０９９９４）；４～２０ｍｇ／Ｌ（ｒ＝０９９９４）。各组分的平均回收率（ｎ＝６）分别为：１００３％，ＲＳＤ＝０４２％；９９７％，ＲＳＤ＝０６９％；９９２％，ＲＳＤ＝０４６％。该法操作简便、快捷，结果准确。     

用色谱-质谱和质量色谱研究苯甲酸钐热分解反应

为合成某些芳香族有机化合物提供一种新途径，用色谱－质谱联用技术和质量色谱法研究了苯甲酸钐的热分解反应产物。其热分解产物溶入丙酮后有大量９，１０－蒽醌析出，其丙酮溶液中还含有１，２－二苯甲酰基苯（２５６％）、苯甲酸（１８７％）、二苯酮（１４４％）、９－芴酮（８２％）、９－苯基芴（４９％）、联苯（３６％）、二苯甲烷（２３％）、３－甲酰苯基联苯（２１％）、二苯基乙二酮（１９％）、４－甲酰苯基联苯（１８％）、芴（１７％）、ｍ－二苯甲酰基苯（１１％）和ｐ－二苯甲酰基苯（０２％）等５５种化合物。讨论了苯甲酸盐的热分解反应机理。     

稀土和氮对灰铸铁耐腐蚀性和抗氧化性的影响

采用包内孕育法研究了稀土和氮对高碳当量灰铸铁耐腐蚀性和抗氧化性的影响。灰铸铁采用中频感应电炉熔炼，化学成分为Ｃ３４％～３５％，Ｓｉ２３％～２４％，Ｍｎ０７０％～０７５％。稀土和氮采用稀土硅铁合金和锰氮铁合金以孕育剂形式加入。研究结果表明，...     

邻苯二甲醛柱前衍生反相高效液相色谱法测定人和小鼠血浆中的游离氨基酸

以邻苯二甲醛（ＯＰＡ）／３－巯基丙酸（３－ＭＰＡ）为衍生试剂，手动柱前衍生，ＯＤＳ（十八基硅烷）柱分离；以磷酸盐缓冲液（ｐＨ７２）配制流动相，二元一级线性梯度洗脱，紫外３４０ｎｍ检测，在４０ｍｉｎ内分离测定了人和小鼠血浆中２１种游离氨基酸的含量。方法准确可靠，２１种氨基酸保留时间和峰面积的相对标准偏差分别为００９％～０３８％和１５％～４９％（ｎ＝８），氨基酸的进样量为０１～１６ｎｍｏｌ时，峰面积与进样量之间的线性相关系数为０９９６～０９９９，标准加入回收率为９３３％～１０５９％。     

用ICP—MS测定高纯氧化镝中痕量稀土元素

考察了源于基体镝的多原子离子干扰。研究了基体对待测稀土杂质信号的影响，采用Ｔｌ内标能基本上补偿基体影响。建立了直接测定高纯氧化镝中痕量稀土杂质的电感耦合等离子体－质谱法。检测限为００１３～００８８μｇ／Ｌ，平均回收率为９２３％～１０１４％，相对标准偏差为２７％～９２％。方法简便、快速、灵敏。     

蜂蜜中四环素族抗生素残留量的薄层色谱测定法

残留在蜂蜜中的四环素族抗生素在经Ｓｅｐ－ＰａｋＣ１８小柱固相萃取处理后，用高效正相薄层色谱予以分离，喷雾显色后用紫外灯进行定性分析；使用双波长薄层扫描仪进行定量测定。在蜂蜜中的添加量为００５０×１０－３、０１０×１０－３及０２０×１０－３时，强力霉素（ＤＣ）、土霉素（ＯＴＣ）和四环素（ＴＣ）的回收率分别为９１６％～１００３％、８４５％～１０３１％和７７０％～１０３２％。该法的测定低限可达到１０－３μｇ。     

流动注射在线预富集—同步扫描荧光法分析水样中痕量多环芳烃

建立了苯并［ａ］芘和的流动注射在线预富集－同步扫描荧光检测法，方法简便快速。苯并［ａ］芘和的测定下限分别为０２μｇ／Ｌ和００４μｇ／Ｌ。测定的相对标准偏差分别为：７１１％和７５４％。用于实际水样的测定，苯并［ａ］芘的回收率为９０％～１０３３％，为１０３３％～１１６７％，结果满意。     

微分脉冲吸附溶出伏安法测定苯胺的研究

苯胺经重氮化、偶合反应定量生成的偶氮化合物具有很强的电活性。作者用微分脉冲吸附溶出伏安法测定偶氮化合物来定量分析苯胺的含量。以ＮＨ３·Ｈ２Ｏ－ＮＨ４Ｃｌ（ｐＨ＝１０）缓冲液为底液，富集电位为－０１５Ｖ，富集时间１２０ｓ，电位扫描速度４ｍＶ／ｓ，在－０６７０Ｖ处产生一个灵敏度高、峰形好的溶出峰。苯胺浓度在１０－９～１０－７ｍｏｌ／Ｌ时与峰电流成线性关系。用印染厂土壤、废水和广州垃圾填埋场的渗出液作标准回收试验，平均回收率分别为９８２％、９７０％、９７５％，测定的相对标准偏差为４３％、４０％、３３％。     

ICP－AES法同时测定高纯碳酸钡中锶钙镁铁

用ＩＣＰＡＥＳ法同时测定高纯碳酸钡中锶、钙、镁、铁考察了谱线选择、基体的影响，确定了仪器最优化工作参数方法回收率为９６—１０７％，ＲＳＤ为４７１－９．６２％     

Preparation of Polystyrene/Triphenyl Phosphate Composites by Suspension Polymerization and Melt Extrusion Method——A Comparative Study

Polystyrene (PS)/triphenyl phosphate (TPP) composites were prepared by both suspension polymerization and melt extrusion, and a comparative study of the flame retardance and mechanical properties was carried out. The results showed that suspension polymerization was a better technique than melt extrusion for obtaining good dispersity of the PS/TPP composite. The TPP nanoparticles, which were approximately 50 nm in size, were homogenously and uniformly dispersed in the PS matrix by suspension polymerization in one-step. However, the PS/TPP composite was partially agglomerated, exhibiting irregularly shaped micron-scale particles as a result of melt extrusion. In contrast to the melt extrusion, the limited oxygen index (LOI) of the PS/TPP nanocomposite by suspension polymerization increased to 22.6% from 21.8%, and time to ignition (TTI) increased by 12.3%, the peak heat release rate (PHRR) decreased by 8.5%, and the total heat release (THR) decreased by 11.0%. The mechanical properties of the PS/TPP nanocomposite by suspension polymerization also increased. The tensile strength, elongation at break, and flexural strength increased by 36.4%, 8.5%, and 108%, respectively.     

双柱吸附法对莲子心总碱的分离纯化研究

研究了大孔吸附树脂和阳离子交换树脂双柱吸附法对莲心碱、异莲心碱和甲基莲心碱的吸附行为。利用阳离子交换树脂D72制备出莲心碱、异莲心碱和甲基莲心碱,含量分别为10.6%、10.6%和28.0%,总含量为49.2%的莲子心总碱提取物,其中杂质主要是水溶性较大的生物碱成分。利用AKS-W大孔吸附树脂能去除极性较大的生物碱,而D72阳离子交换树脂能去除非生物碱的特点,采用双柱联合吸附法,制备出3种吸附质含量分别为33.1%、15.0%和34.5%,总含量为82.6%的莲子心总碱提取物。     

追风伞挥发油的化学成分研究

 研究了贵州产追风伞 (LysimachiatrientaloidesHemsl.)挥发油的化学成分。采用水蒸汽蒸馏法提取追风伞挥发性成分 ,用气相 质谱进行分离测定 ,结合计算机质谱图库检索技术对分离的化合物进行结构鉴定 ,从中鉴定出 4 0种化学成分 ;应用峰面积归一化法测定各成分的相对含量。水蒸汽蒸馏提取物的提取率是 0 11%。研究结果表明 ,贵州产追风伞挥发油的主要成分为萜烯类及其含氧衍生物等 ,主要有广藿香醇 (2 2 5 4 % )、乙酸龙脑酯(16 17% )、γ 古芸烯 (3 2 7% )、δ 愈创烯 (2 6 2 % )、橙花叔醇 (2 0 2 % )、芳樟醇 (1 99% )和棕榈酸 (1 96 % )。     

Antimicrobial activity and chemical constituents of the essential oils from flower, leaf and stem of Gypsophila bicolor from Iran

The volatile constituents from flower, leaf and stem of Gypsophila bicolor growing in Iran were obtained by hydrodistillation and analyzed by GC and GC/MS. The flower oil was characterized by high amounts of germacrene-D (21.2%), p-cymene (20.6%), bicyclogermacrene (17.6%), gamma-dodecadienolactone (13.7%) and terpinolene (9.4%). Twenty-four constituents representing 97.4% of the leaf oil were identified of which germacrene-D (23.4%), terpinolene (14.5%), bicyclogermacrene (7.5%), gamma-dodecadienolactone (6.8%), p-cymene (6.7%) and cis-beta-ocimene (6.3%) were major components. The main components of the stem oil were gamma-dodecadienolactone (28.5%), bicyclogermacrene (14.8%), germacrene-D (12.6%), p-cymene (12.5%), terpinolene (11.6%) and trans-beta-ocimene (4.2%). The antimicrobial effects of flower, leaf and stem essential oils from Gypsophila bicolor were studied according to the agar diffusion cup method. The essential oils had a moderate effect on the Gram-positive and Gram-negative bacteria, but had a substantial effect on the fungi studied.     

高效液相色谱法测定藻类中的类胡萝卜素和叶绿素

提出了用高效液相色谱法测定藻类中类胡萝卜素和叶绿素的方法。采用丙国等有机溶剂提取藻类中的类胡萝卜素和叶绿素,然后在反相C18柱上进行分离。流动相选用二氯甲烷／乙腈／甲醇／水（22.5:9.5:67.5:0.5）,流速为1.0mL／min。用光度检测器检测报长为450um。叶黄素、α-胡萝卜素、β-胡萝卜素、叶绿素a和叶绿素b的平均回收串分别为99.1％,98.5％,99.4％,100.6％和99.9％,相对标准偏差分别为2.4％,5.6％,6.0％,4.1％和4.0％。     

缓释尿素中硝化抑制剂DMPP的气相色谱法测定

建立了一种检测缓释尿素中吡唑类硝化抑制剂DMPP的气相色谱法。DMPP在尿素水溶液中可定量转化为DMP,从5种有机溶剂中选择氯仿作为DMP的萃取剂,并采用加入KCl盐析的方法将萃取率从96.1%提高到99.5%。本文采用吡啶作为内标物,通过DB-1701气相色谱柱,氢火焰离子化检测器(FID)定量检测氯仿溶液萃取相中的DMP。萃取率为98.8%~100.4%;添加回收率为98.1%~99.5%;RSD为0.84%~1.6%。应用本法测定自制缓释尿素中DMPP质量分数为0.44%。     

2,3-二甲基-4-氯吡啶-N-氧化物的合成工艺改进

对2,3-二甲基-4-氯吡啶-N-氧化物(4)的合成工艺进行了改进。以2,3-二甲基吡啶为原料,经氧化(钨酸钠为催化剂,双氧水为氧化剂,收率96.5%),硝化(65%的浓硝酸为硝化剂,收率86.3%,纯度99.0%)及氯化(乙酰氯为氯化剂,收率86.8%,纯度98.6%)合成了4,总收率72.2%,4的结构经1H NMR表征。     

ISOLATION AND PURIFICATION OF ALKALOIDS FROM PLUMULA NELUMBINIS BY DOUBLE-COLUMN ADSORPTION CHROMOTOGRAPHY

The performance of adsorption and separation for liensinine, isoliensinine and neferine was studied by double-column adsorption chromatography using macroporous adsorption and cation exchange resins. The alkaloid extract with 49.2% total contents by mass representing 10.6% liensinine, 10.6% isoliensinine and 28.0% neferine respectively was prepared by D72 cation exchange resins, in which most of the impurities were water-soluble alkaloids. Furthermore, the alkaloid extract with 82.6% total contents by mass containing 33.1%, 15.0% and 34.5% of the three adsorbates respectively was prepared by double-column adsorption chromatography using AKS-W macroporous adsorption and D72 cation exchange resins. As a result, the content of single and total alkaloids has been greatly increased by the double-column adsorption chromatography.     

顶空固相微萃取-气相色谱-质谱法用于白术中挥发性成分的分析

采用顶空固相微萃取-气相色谱-质谱法(HS-SPME-GC-MS)分离鉴定了白术中的挥发性成分,并与采用传统的水蒸气蒸馏法(SD)提取的挥发性成分进行了比较。实验中筛选了固相微萃取纤维头,优化了SPME的操作条件。样品在70 ℃下平衡30 min后,用65 μm聚二甲基硅氧烷-二乙烯基苯(PDMS-DVB)纤维头对白术样品顶空吸附30 min,于250 ℃下解吸4 min, 然后采用GC-MS对解吸物进行分离鉴定;采用HS-SPME-GC-MS鉴定出41种组分,占总峰面积的90.81%;采用SD-GC-MS鉴定出31个组分,占总峰面积的88.19%,且采用SD所提取的组分基本上都被固相微萃取所提取。结果表明, HS-SPME可取代耗时的SD用于白术中挥发性物质的提取。     

Effects of stereo-regularity of multiblock co-poly(rac-lactide)s on stereo-complex microparticles and their insulin delivery

Uniform stereo-complex microparticles ranging from nanometer to micrometer size are prepared by using stereo multiblock co-poly(rac-lactide)s (smb-PLAs) with different stereo-regularity. At comparable molecular weights, as the smb-PLA stereo-regularity decreases from 88% to 76%, the crystallinity of the microparticles decreases noticeably, as proved by DSC and WAXD. At the same time, the shape of the microparticles varies from the flower shape to the sphere shape and the particle size increases markedly from 700-2700 nm as shown by SEM. However, all insulin-loaded microparticles are of cake-shape and their sizes depend on the stereo-regularity. The crystallization of smb-PLAs facilitated by insulin is evidenced by the increase of T(m) and DeltaH(f) in DSC. The highest insulin-loading content of 14.2% and -entrapment efficiency of 82.8% are obtained from the smb-PLA with the highest stereo-regularity of 88%. Release studies in vitro show the least first-day release at about 25% followed by continuous release of another 70% of insulin over one month. Stereo-complex microparticles of smb-PLAs with lower stereo-regularity resulted in a relatively lower insulin-entrapment efficiency and -loading content, a larger first-day release, and also complete release of 90% of the total amount within one month. The release system follows a diffusion mechanism. By contrast, atactic PLA shows a very low entrapment efficiency of 16.7%. Structure of a stereo multiblock co-poly(rac-lactide).