Determination of 5-fluorouracil in plasma and whole blood by ion-pair high-performance liquid chromatography

5-Fluorouracil in blood or plasma was determined by extraction and column liquid chromatography. Acetonitrile was added to blood or plasma and the mixture was stirred and centrifuged. Zinc sulfate addition was followed by stirring and centrifuging. The acetonitrile was salted out with ammonium sulfate, and an aliquot was evaporated with nitrogen. The residue was dissolved in mobile phase and chromatographed. The stationary phase was a styrene-divinylbenzene copolymer, and the mobile phase was 10 mM tetrabutylammonium hydroxide-methanol (74:26). 5-Fluorouracil was detected by UV absorption at 266 nm. Time of the assay was less than 30 min. The detection limit was 10 ng/ml and the relative standard deviation was 4 to 10% depending on the concentration.     

基体辅助激光解吸电离飞行时间质谱用于人参皂甙Rg3的定量分析

考察了基体辅助激光解吸电离时间飞行质谱用于人参皂甙Rg3 定量分析时内标的选择。加入棉子糖作为内标时 ,Rg3 的定量标准曲线的回归系数R2 =0 .938,平均相对误差为 2 8 6 % ;加入性质相近的芦丁后 ,Rg3 的定量标准曲线的回归系数R2 =0 993,平均相对误差为 7 5 %。分辨率的提高以及采用Rg3 和内标物的质谱峰的相对面积来代表Rg3 的浓度可以使定量的重现性明显改善     

Electro-responsive polyacrylamide-grafted-gum ghatti copolymer for transdermal drug delivery application

An application of polyacrylamide-grafted-gum ghatti (PAAm-g-GGH) copolymer for transdermal delivery of an anti-psychotic drug, quetiapine fumerate triggered by electric stimulus was explored. The electro-responsive PAAm-g-GGH was prepared by free radical polymerization underneath nitrogen atmosphere subsequent to alkaline hydrolysis. The PAAm-g-GGH was used as drug reservoir gel and crosslinked films of GGH and PVA as rate controlling membranes (RCM). The reservoir gels were uniform and translucent; pH of gels was 6.56–7.06, which is in the pH range of skin and drug content was from 89.57% to 94.51%. The thickness of RCMs was 163–227?μ; thickness was increased with increased glutaraldehyde concentration and all the RCMs were permeable to water vapors. When electric stimulus was absent, a small amount of drug was permeated from the formulations, while drug conveyance was enhanced in the existence of stimulus. Drug permeation was increased with increase in electric stimulus from 2 to 8?mA. Over two fold increase in flux was observed after application of electric stimulus. Under “on–off” electric stimulus, faster drug permeation was seen under ‘on’ condition and permeation was decreased when stimulus was ‘off.’ Histopathology study confirmed reversible alteration of skin structure under electric stimulus.     

亲水相互作用色谱柱串联C18柱高效分析饮品中的胭脂红

建立了亲水相互作用色谱柱(HILIC)串联C18柱的方法,高效分离实际样品中的胭脂红,并对色谱柱的串联顺序以及色谱分离条件进行优化。结果表明:当HILIC柱在前C18柱在后,流动相为乙腈-乙酸铵(5 mmol/L)=91∶9(V/V),流速为0.9 mL/min,柱温为25℃,检测波长为508 nm时,此时胭脂红的分离效果最佳。在最佳的色谱分离条件下,选用两种市售饮品进行实际样品的测定,回收率在81.2%~119%。方法适用于水相样品中的强极性物质的高效分离与分析。     

植物油酸新戊二醇对苯二甲酸复合酯的合成及性能

用新戊二醇(NPG)和对苯二甲酰氯(TPA)反应生成“低聚物”中间体,当n(NPG)/n(TPA)由2.4增加至3.0时,中间体的聚合度(m)在3.5~1.45之间,收率75.5%。再将中间体与油酸、菜籽油酸进行酯化得到复合酯,收率88.5%。结果表明,复合酯的粘度随着分子量的增大而增大,粘度指数大于125,凝点低于－27℃,氧化稳定性随分子量的增大而提高,生物降解率＞70%,最大无卡咬负荷(PB)为784N,磨斑直径0.41mm,热分解温度＞250 ℃,因此植物油酸新戊二醇对苯二甲酸复合酯是性能良好的绿色润滑剂。     

高效液相色谱法测定葛根芩连片中的葛根素

建立高效液相色谱测定葛根芩连片中葛根素含量的方法。以体积分数50%的甲醇为提取液对样品超声提取20 min,采用DiamonsilTMC18(250 mm×4.6 mm,5μm)色谱柱,以甲醇–乙腈–水(体积比8∶12∶80)为流动相,流速为1.0 mL/min,检测波长为250 nm,柱温为30.0℃,进样量体积10μL。在最佳实验条件下,葛根素与其它物质能完全分离,葛根素的质量浓度在5.43~543.2μg/mL范围内与色谱峰面积呈良好的线性,线性相关系数r=0.999 9,方法检出限为3.50μg/mL(S/N=3)。方法加标回收率为100.0%,测定结果的相对标准偏差为1.6%(n=6)。该方法简单、快速、重现性好,适用于葛根芩连片中葛根素的测定。     

高效液相色谱–光电二极管阵列法测定虾青素的含量

建立虾青素含量测定的高效液相色谱–光电二极管阵列法。采用Purospher STAR RP 18(4.6 mm×250mm,5μm)色谱柱,以甲醇–水(体积比为95∶5)为流动相,流速1.0 mL/min,检测波长为482 nm,柱温为30℃,进样量为20μL。在所选定的液相色谱条件下,虾青素主峰与其它杂质峰分离良好,虾青素在0.2~16μg/mL范围内线性良好,线性相关系数r=0.999 9,检出限为0.01μg/mL,测定结果的相对标准偏差为0.42%(n=6),平均回收率为100.4%。该法分析快速准确、灵敏度高、重现性好。     

穿心莲内酯的溶剂浮选

应用溶剂浮选法对穿心莲乙醇提取液中的穿心莲内酯进行分离富集,优化了穿心莲内酯的浮选条件.实验表明:浮选溶剂为乙酸乙酯,水相与有机相体积比为2: 1,加入水相体积4%的乙醇,溶液pH 7,氮气流速200 mL/min,浮选时间40 min为最佳浮选条件.在最佳实验条件下,穿心莲内酯平均收率为94.1%; RSD为1.1%,平均标准加入回收率95.1%; 富集倍数为9.7倍.溶剂浮选法分离穿心莲内酯不仅能得到满意的回收率和富集倍数,并能有效地除去水溶性杂质,提高目标物纯度.与溶剂萃取法相比, 溶剂浮选法能节约有机溶剂和操作时间.     

Determination of bencyclane in human plasma by means of capillary gas chromatography and nitrogen-phosphorus selective detection

A sensitive and specific method for the determination of bencyclane in human plasma is presented. Bencyclane was extracted from human plasma with two 3-ml volumes of isooctane and was shaken for 10 min. The organic phase was separated and evaporated to dryness at 40 degrees C under a nitrogen stream. The residue was dissolved and an aliquot was injected into the gas chromatograph. The separation was performed with a DB-17 column with helium as the carrier gas. Nitrogen-selective detection was performed. The quantification was performed with the signal output. The limit of detection was 1 ng/ml.     

松香改性酚醛环氧树脂的合成与表征

以松香,环氧氯丙烷,甲醛及苯酚等为主要原料,合成了一种新型的环氧树脂。通过正交实验法确定了环氧化反应的最佳实验条件,即环氧化温度90℃,碱用量13 g,催化剂为cat 1,其最佳用量为0.018 mol,环氧氯丙烷的用量为50 g,碱浓度为30%(以上数值均以松香用量为70 g时计)。在最佳实验条件下合成得到了松香改性酚醛环氧树脂(简称RAPE),并用HPLC、FT-IR、NMR对其进行结构表征。结果表明,得到的RAPE其环氧值为0.28 mol/100g,平均聚合度约为3.4,酚羟基和树脂酸上的羧基基本反应完全,得到一种新型的缩水甘油醚型和缩水甘油酯型的环氧树脂。     

Dissolution and bioavailability of phenobarbital in solid dispersion with phosphatidylcholine.

The dissolution of phenobarbital (PB) from solid dispersion with phosphatidylcholine (PC) was studied. PB was present in an amorphous state in solid dispersion (PB-PC) if the mole fraction of PB was under 0.75. Thus, supersaturation was observed when an excess amount of PB-PC was dispersed in pH 1.2 and 6.8 media. The degree of supersaturation was largest when the mole fraction of PB was 0.25, although it was only 1.3-fold of the PB solubility in this case. Dissolution from PB-PC was rapid and complete in both pH 1.2 and 6.8 media regardless of the mole fraction of PB, above 90% within 5 min. Bioavailability after the oral administration of PB-PC to rabbits with a dose of 15 mg/kg equivalent to PB was compared with that of PB crystals. The area under the plasma concentration curve was bigger, but not significant. The maximum concentration was significantly higher, and the time to maximum concentration was significantly faster. These results indicate that the absorption rate became high with PB-PC because the dissolution was rapid.     

模拟首饰佩戴中有害元素释放量的研究

建立首饰佩戴动态磨损模型,对首饰磨损过程中有害元素的迁移进行了研究.用原子吸收光谱法测定有害元素释放量,发现在模拟首饰佩戴过程中,佩戴时间越长,有害元素的释放量越大,释放量随时间的增加基本呈线性增长;80％的有害元素在日常磨损过程中离子化;饰品日常佩戴磨损过程中有害元素的释放量是饰品直接释放量的40％.     

动态超声辅助萃取与HPLC联用测定淫羊藿中黄酮类化合物

建立了动态超声辅助萃取与高效液相色谱在线联用系统,用于测量淫羊藿中黄酮类化合物。萃取过程在一个循环体系中完成,萃取完成后,通过采样环采集20μL萃取液,萃取液被流动相载入色谱系统进行分离检测。4种黄酮类化合物用HPLC–MS区分,通过比较色谱峰面积选择优化萃取条件。选择50℃的水浴温度,50%的乙醇作为萃取剂,萃取剂流速为1.5 mL/min,萃取时间为8 min,样品量为15 mg。用该法测量淫羊藿样品中4种黄酮类化合物,日内、日间精密度分别为1.05%～2.05%,0.30%～3.63%(n=6)。淫羊藿中的主要化合物淫羊藿苷的加标回收率为95.2%。该方法可用于测量淫羊藿中的黄酮类化合物。     

ICP–OES法测定八氧化三铀中杂质元素钨

以ICP–OES法测定八氧化三铀中杂质元素钨。采用浓HNO3–浓HCl、浓HNO–HF、3 mol/L HNO3三步酸溶方案,利用CL–TBP萃淋树脂将铀基体分离,淋洗液基质为3 mol/L HNO3,淋洗液流速为1 mL/min。弃去最初2 mL死体积淋洗液后接收10 mL,分离回收率平均值为95.93%,线性方程为y=539.71x+16.6,相关系数r2=0.999 7,4水平样品测定结果的相对标准偏差为0.39%~3.12%(n=6)。用该方法对标准物质进行测定,测定结果在参考值范围内。     

Dawson型磷钨酸催化合成乳酸月桂醇酯

用Dawson型磷钨酸催化合成乳酸月桂醇酯。实验结果表明:Dawson型磷钨酸有较高的催化活性,反应时间短,酯收率高,工艺简单。最佳工艺条件为:醇/酸摩尔比为1.5:1,催化剂用量为0.3%,带水剂甲苯体积(mL)与反应物质量(g)之比为0.4:1~0.5:1,反应温度为115~140℃,反应时间30~50min。在此条件下,酯收率可超过93% 。     

含DNA配体的VT吸附剂结构及其血液相容性研究

 本文以异氰尿酸三烯丙酯 TAIC)为交联剂,醋酸乙烯酯(VAC)为单体合成的共聚物(VT),经皂化和活化后,固载上DNA,即得含DNA配体的VT吸附剂。测定了各产物的物理性能,表面形态,红外光谱和血液相容性。实验结果表明:聚合物具有较大平均孔径,皂化后亲水性增强,随活化而使比表面积增大,孔分布趋于均匀,固载DNA的能力高,致使最后产物表面DNA覆盖致密程度高,考察其血液相容性良好,对血小板粘附率约为10％,对白细胞无破坏,每克吸附剂清除抗-DNA蛋白2小时可达60％以上。     

海藻酸钠-壳聚糖微胶囊膜强度的研究

以乳化/内部凝胶化法制备了海藻酸钠-壳聚糖微胶囊,重点考察了成膜反应过程中影响微胶囊膜强度的几个主要参数,实验发现,壳聚糖分子量低于100000,成膜反应时间高于15min,壳聚糖溶液pH值在6.0左右时制备的微胶囊膜强度较高.初步探讨了海藻酸钠与壳聚糖两种高分子发生聚电解质络合反应的机制.     

表面活性剂协同微波提取紫背天葵色素的研究

从紫背天葵(begonia fimbristipula hance)中提取了紫背天葵色素,并优化了提取条件;提取剂为0．03％(w)的K12-45％(φ)乙醇水溶液,用量为每克原料加入30mL提取剂,微波功率为464w,提取时间为200s,提取次数为2次提取率为94．8％,产率为9．31％;色价E(1％,510nm)为23．7．产品pH值为6．4与溶剂浸提法相比,每次提取时间减小36倍,提取率增加22．3％。     

F离子掺杂TiO2的性能研究

以NH₄F为掺杂剂,采用溶胶-凝胶法制备F离子掺杂型TiO₂光催化剂,对其进行XRD、XPS和PL表征,结果表明,F离子掺杂TiO₂由于Ti-F配位体的形成而能抑制金红石相的生成,同时F离子掺杂能增加TiO₂表面缺陷浓度并降低Ti_2P键的结合能,另外,由于F离子能取代Ti-OH配位体而降低了表面羟基氧浓度.光催化研究结果表明,F离子掺杂提高了TiO₂光催化活性近1.5倍.     

Extraction and separation of cationic surfactants from river sediments: application to a spectrophotometric determination of cationic surfactant in an aquatic environment using membrane filters.

The quantitative extraction of cationic surfactant (CS+) in river sediments was studied. Further, the developed method was applied to the spectrophotometric determination of CS+ in urban river sediment samples by solid-phase extraction with membranes. A mixture of methanol and hydrochloric acid was proposed as an eluent. Dried sediment was digested in the eluent under ultrasonic irradiation. After elution, the eluent was evaporated to almost dryness. The residue was dissolved in a small volume of methanol and diluted to a certain volume with water. The pH of the solution was adjusted to 4-5 to separate iron and some other metals as precipitates of hydroxides. The solution was passed through two-piled membranes: first glass-fiber and then polytetrafluoroethylene (PTFE) membranes. A small volume of methanol was passed through the membranes to elute any CS+ retaining on the membranes. After passing the methanol solution through a cationic exchange resin column, the retained CS+ was eluted with methanol containing a high concentration of sodium chloride. Water, Bromophenol Blue (BPB) and hydrochloric acid were added to the solution. The solution was passed through a mixed cellulose ester membrane filter to retain an ion associate of CS+.BPB-. The retained ion associate was dissolved in a small volume of N,N-dimethylformamide together with the membrane filter, followed by the addition of triethanolamine to make the solution alkaline. The absorbance due to BPB2- was measured at 603 nm against a reagent blank. This method was applied to the determination of CS+ in river water and sediment. A cationic surfactant in sediments at 10(-5) mol kg-1 levels was detected with satisfactory precision. It was found that CS+ was about 500-fold enriched in the sediment from water at the place where domestic wastewater was discharged.