杏仁油的物化性能及其脂肪酸组成的分析

用３种不同溶剂萃取杏仁得到杏仁油,并对其物化常数进行测定。杏仁油用饱和氢氧化钾 甲醇皂化,再用甲醇 硫酸（体积比为４∶１）甲酯化后,将乙醚萃取液作气相色谱分析。太原杏仁油中脂肪酸的主要成分为油酸（Ｃ１８∶１,质量分数约６８％）和亚油酸（Ｃ１８∶２,质量分数约２５％）,少量棕榈酸（Ｃ１６∶０）、棕榈烯酸（Ｃ１６∶１）和硬脂酸（Ｃ１８∶０）,微量花生酸（Ｃ２０∶０）。     

HPLC法测定中成药制剂中10-羟基-2-癸烯酸的含量

采用ＳｐｈｅｒｉｓｏｒｂＣ１８柱,以甲醇∶水∶磷酸（４５∶６５∶０．５）为流动相,以ＵＶ２１０ｎｍ为检测波长,测定中成药制剂中１０－羟基－２－癸烯酸（１０－ＨＤＡ）的含量,１０－ＨＤＡ浓度在０．００６～０．０３０ｇ／Ｌ范围内线性关系良好（ｒ＝０．９９９９,ｎ＝５）,检测限为０．２ｍｇ／Ｌ（Ｓ／Ｎ＝３∶１）。方法具有定量准确、快速及主峰和杂质分离度高等特点。     

花生中黄曲霉毒素B1、B2、G1、G2的多功能净化柱-高效薄层色谱分析

建立了一种测定食品中黄曲霉毒素（ ＡＦＴ） Ｂ１ 、Ｂ２ 、Ｇ１ 、Ｇ２ 的多功能净化柱（ ＭＦＣ） 净化, 单相展开的薄层色谱法。 以乙腈－ 水（ 体积比９ ∶１） 提取样品中ＡＦＴ, 经ＭＦＣ 净化浓缩后, 采用ＨＳＧ６０ 薄层板, 以丙酮－ 氯仿（ 体积比９ ∶１） 展开, 薄层扫描仪荧光检测扫描定量。该法用于花生样品的检测,４ 种毒素的分离良好; 线性范围：０ ．０５ ～１ ．０ ｎｇ, 相关系数≥０ ．９９９ １; 检出限均达到０ ．５ ×１０ － ９ ; 相对标准偏差为４ ．６７ ％ ～１０ ．２１ ％ ; 样品加标０．５ ×１０ － ９ ～１０ ×１０ － ９ , 平均回收率为８６ ．５ ％ ～９９ ．０％ 。     

毛细管气相色谱法测定水体及土壤中溴氟菊酯农药的残留量

建立了新品农药溴氟菊酯在水体及土壤中残留量的测定方法，采用石油醚＋丙酮（３＋１）混合溶剂提取，经浓硫酸＋无水乙醇（１＋１）纯化，用毛细管气相色谱电子捕获检测器测定。该法检出限为０．１×１０－９～２×１０－９，回收率７２．６％～１００．５％，变异系数１．６％～８．５％。     

花生中多菌灵残留量的高效液相色谱分析方法的研究

建立了测定花生中多菌灵残留量的高效液相色谱法，以乙酸乙酯提取，乙腈萃取分离，石油醚去酯，乙醇＋水（４＋１）沉淀蛋白质，在Ｒａｄｉｌ＿ＰａｋＣ１８柱上，甲醇＋水（５５＋４５）为流动相，采用外标法进行定量检测，相对标准偏差为０１８％，回收率在８００％～９８０％，最低检测限为０２ｍｇ／Ｌ。     

用亚硝基R盐螯合树脂分离富集催化极谱法测定矿石中的铱

本文研究了利用亚硝基Ｒ盐螯合形成的树脂，分离富集试液中痕量贵金属元素铱的实验条件。并利用ＪＰ－１型示波极谱仪，在１．５０ｍｏｌ／Ｌ盐酸＋５．０×１０＾－５ｍｏｌ／Ｌ硫脲＋０．２ｍｏｌ／Ｌ盐酸＋５．０×１０＾－５ｍｏｌ／Ｌ硫脲＋０．２ｍｏｌ／Ｌ碘化钾＋碲（ρ（Ｂ）＝０．４ｍｇ／Ｌ）的混合底液中，对铱进行极谱催化波测定。在示波极谱仪上峰电位约－０．５５Ｖ（银汞齐为参比电极），可测定试液中５．０×１．０     

新显色剂2-(5-羧基-1,3,4-三氮唑偶氮)-5-二乙氨基酚的合成及其与铋的显色反应

首次合成了新显色剂２－（５－羧基－１，３，４－三氮唑偶氮）－５－二乙氨基酚（简称ＣＴＺＡＰＮ），研究了它的性质及其与铋显色反应的条件。结果表明：试剂的分子式Ｃ１３Ｈ１６Ｎ６Ｏ３分子量３０４．３２，ｍ．ｐ． ２５２℃，各级酸离解常数为ＰＫａ１＝３．１，ＰＫａ２＝７．５，ＰＫａ＝９．６；在ＰＨ ７的 ＮＨ４Ａｃ介质中，试剂与铋形成紫红色络合物，λｍａｘ为 ５４０ ｎｍ，对比度△λ为 １２０ ｎｍ，络合比Ｂｉ３＋：Ｒ＝１：２，摩尔吸光系数５．１３ ×１０４Ｌ·ｍｏｌ－１·ｃｍ－１，Ｂｉ３＋在０～１．８ ｍｇ／Ｌ范围内遵守比耳定律，在掩蔽剂的作用下，可不经分离直接测定合金样品及合成工业废水中微量铋，结果满意。     

掺Eu3+离子Y2SiO5晶体格位选择光谱研究

分别利用白光灯、４５７－９ ｎｍ 氩离子激光、二倍频ＹＡＧ∶Ｎｄ 激光泵浦的诺丹明６Ｇ 可调谐窄线宽（０－５ ｃｍ －１） 染料激光作为光源， 以单色仪锁相放大器光电倍增管计算机数据采集系统记录光谱， 测量并研究了Ｙ２ＳｉＯ５∶Ｅｕ３ ＋ 晶体的透射光谱、荧光光谱、激发光谱和格位选择荧光光谱。５Ｄ０ →７Ｆ０，１ ，２ ，３，４ 跃迁，３０ 多根谱线（总数为５０ 根） 被观察到。在该晶体中Ｅｕ３＋ 替换Ｙ３＋ 离子， 占据两个较低对称性的光学格位， 这两个格位的５Ｄ０ ７Ｆ０ 能级跃迁谱线相隔大约只有０－２ ｎｍ ， 在室温下有一定的光谱关联。并用Ｘ射线谱对晶体的晶格常数ａ ， ｂ，ｃ 和晶面角度β进行测量， 测量结果显示掺杂后的晶格常数和未掺杂的Ｙ２ＳｉＯ５ 晶格常数基本一致。     

蛇鞭的化学成分研究Ⅱ.以色质联用技术鉴定黑眉锦蛇蛇鞭的油状物和脂肪酸组成

通过溶剂萃取和柱色谱分离，从黑眉锦蛇蛇鞭中分离得到５个油状物及混合脂肪酸样品。用气相色谱－质谱－计算机联用技术鉴定了油状物中的５，８，１１，１４－花生四烯酸乙酯、９－十八碳烯－１－醇、４－丙基－苯酚、Ｎ－苯基－２－萘胺、３－烯基－２－己酮等１８种化学成分。并鉴定了２３种脂肪酸，其中饱和脂肪酸１０种，不饱和脂肪酸１２种，芳香酸１种；发现存在着多种自然界少见的奇数碳脂肪酸和支链酸。     

蛇鞭的化学成分研究：II.以色质联用技术鉴定黑眉锦蛇蛇鞭的油状物 …

通过溶剂萃取和柱色谱分离，从黑眉锦蛇蛇鞭中分离得到５个油状物及混合脂肪酸样品。用气相色谱－质谱－计算机联用技术鉴定了油状物中的５，８，１１，１４－花生四烯酸乙酯、９－十八碳烯－１－醇、４－丙基－苯酚、Ｎ－苯基－２－萘胺、３－烯基－２－己酮等１８种化学成分。并鉴定了２３种脂肪酸，其中饱和脂肪酸１０种，不饱和脂肪酸１２种，芳香酸１种；发现存在着多种自然界少见的奇数碳脂肪酸和支链酸。     

Chemical Studies of Formosan Cobra (Naja Naja Atra) Venom. Part V. Properties of 5′-Nucleotidase

The chromatographically, disc and microzone electrophoretically homogeneous 5′-nucleotidase of Formosan cobra venom was prepared. This enzyme has molecular weight of about 10,000 as estimated by gel filtration and by total amino acid analysis. Maximal activity was exhibited between pH 6.5 and 7.0 in 0.1 M Tris-malonate buffer. Mn⁺⁺ and Mg⁺⁺ ions enhance the activity. The maximal enhancement was obtained at the final concentration of 10^?3 M regardless of substrate concentration. Ni⁺⁺ and Zn⁺⁺ ions inhibit the activity. It is heat stable up to 50° C for 2 min but complete inactivation occurs at 80° C. It shows a high specificity for hydrolysis of ribonucleoside-5′-phosphate but shows only 20% and completely inactive to deoxyribonucleoside-5′-phosphate and 2′-or 3′-nucleotide, respectively. Apparent Km and Vmax values were also determined for AMP, GMP, UMP and CMP.     

Chemical Studies of Formosan Cobra (Naja Naja Atra) Venom Part IV. Estimation of molecular weights of some purified protein fractions by sephadex gel filtration

Molecular weights of four purified fractions, Fractions VIII (cobraneurotoxin), IX (5′-nucleotidase), XI (cardiotoxin) and XII (cardiotoxin) of Formosan cobra venom were estimated by gel filtration on Sephadex G-100 and G-75 columns.     

Chemical Studies of Formosan Cobra (Naja Naja Atra) Venom: Part II. Isolation and Characterization of Guanosine,Adenosine, and Inosine from Cobra Venom

A non-protein fraction from crude Formosan cobra venom was found to be a nucleoside mixture. The components were identified as guanosine, adenosine and inosine by paper chromatographic and polyamide thin-layer chromatographic correlations and their spectroscopic data. The mole ratio of guanosine/adenosine/inosine was found to be 7:2.5:1.     

Chemical Studies of Formosan Cobra (Naja Naja Atra) Venom: Part III. N-Terminal Amino Acid Analysis of Some Purified Protein Components by DNP and DNS Methods

N-Terminal amino acid residues of Fractions IX, X, and XII were reinvestigated by DNP and DNS methods with two-dimensional polyamide thin-layer chromatography. It was found that our previous work¹ had been erroneously concluded. By the present work, it was obvious that all three fractions had Leu as their N-terminal amino acid residues.     

Antihaemorrhagic potentials of Fagonia cretica against Naja naja karachiensis (black Pakistan cobra) venom

Plants have been extensively used as a remedy for the treatment of snake bites. The aim of this study was to determine the antivenom potentials of methanolic extract from the aerial parts (leaves and twigs) of Fagonia cretica L. on a haemorrhage induced by venom from Naja naja karachiensis. The haemorrhagic response of venom was dose dependent from 0.1 to 4.0?μg per 1.5?μL phosphate buffer saline (PBS) on vitelline veins of fertilised hens' eggs in their shells. The extract effectively eliminated and neutralised, in a dose-dependent manner, the haemorrhagic activity of snake venom. The minimum effective neutralising dose of F. cretica extract was found to be 15?μg per 1.5?μL PBS. The extract possesses potentials as haemorrhagic inhibitor against snake venom compared to the standard antiserum and various plants reported in the literature. This study also provides a scientific base for the use of F. cretica in traditional medicine for the treatment of snake bite.     

A strategy for the enrichment and characterization of disulfide bond-contained proteins from Chinese cobra (Naja atra) venom

A new strategy combined gold-coated magnetic nanocomposites assisted enrichment with mass spectrometry was developed for the characterization of disulfide bond-contained proteins from Chinese cobra (Naja atra) venom. In this work, core-shell nanocomposites were synthesized by the seed-mediated growth method and used for the enrichment of snake venom proteins containing disulfide bonds. A total of 3545 tryptic digested peptides derived from 96 venom proteins in Naja atra venom were identified. The venom proteins comprised 14 toxin families including three-finger toxins, phospholipase A₂, snake venom metalloproteinase, cobra venom factor, and so forth. Extra 16 venom proteins were detected exclusively in the nanocomposites set, among which 11 venom proteins were from the three-finger toxins family. In the present study, the proposed simple and efficient protocol replaced the tedious and laborious technologies commonly used for pre-separating crude snake venom, suggesting widely implementation in low-abundance or trace disulfide bond-contained proteins or peptides characterization.     

Effects of 3FTx Protein Fraction from Naja ashei Venom on the Model and Native Membranes: Recognition and Implications for the Mechanisms of Toxicity

Three-finger toxins are naturally occurring proteins in Elapidae snake venoms. Nowadays, they are gaining popularity because of their therapeutic potential. On the other hand, these proteins may cause undesirable reactions inside the body′s cells. A full assessment of the safety of Naja ashei venom components for human cell application is still unknown. The aim of the study was to determine the effect of the exogenous application of three-finger toxins on the cells of monocytes (U-937) and promyelocytes (HL-60), with particular emphasis on the modification of their membranes under the influence of various doses of 3FTx protein fraction (0–120 ng/mL). The fraction exhibiting the highest proportion of 3FTx proteins after size exclusion chromatography (SEC) separation was used in the experiments. The structural response of cell membranes was described on the basis of single-component and multi-component Langmuir monolayers that mimicked the native membranes. The results show that the mechanism of protein–lipid interactions depends on both the presence of lipid polar parts (especially zwitterionic type of lipids) and the degree of membrane saturation (the greatest-for unsaturated lipids). The biochemical indicators reflecting the tested cells (MDA, LDH, cell survival, induction of inflammation, LD50) proved the results that were obtained for the model.     

Chemical Studies of Formosan Cobra (Naja naja atra) Venom. Part I. Chromatographic Separation of Crude Venom on CM-Sepadex and Preliminary Characterization of its Components

The crude venom of Formosan cobra (Naja naja atra) was separated into 12 fractions by CM-Sephadex (C-50) chromatography with ammonium acetate buffer by two-stage gradient elution. Fr. I was proved to be a mixture of nucleotides and nucleosides. The toxicity was found in Fr. VIII (neurotoxic), X (cardiotoxic), XI (cardiotoxic), and XII (cardiotoxic). Glycerophosphatase, alkaline phosphomonoesterase, and 5′-nucleotidase were found in Fr. III, V and IX, respectively. Phosphodiesterase was distributed in Frs. VI and VII, while lecithinase-A (phospholipase-A) was found in Frs. IV and V. Frs. VIII, IX and XII seem to be homogenous by the n-terminal analysis and the paper electrophoresis.