麝香系统溶液结晶溶剂选择的研究

从分子结构和分子间力的角度在理论上推测了酮麝香系统（酮麝香、二甲苯麝香、乙酰化物）在某些溶剂中的溶解性能,为进一步选择结晶用溶剂奠定了基础,经实验验证,理论预测与实验基本相符。首次提出以克溶质／一定分子数的溶剂表示溶解度,它能从本质上反映分子之间作用力的大小。     

略谈两类重要的动物香料及其合成

本文综述了龙涎香及麝香两类动物香料合成方法的进展,并就保护和合理利用自然资源提出了个人的意见。     

气相色谱-质谱联用法快速检测乳类化妆品中6种合成麝香

目的建立同时、快速测定化妆品中葵子麝香、佳乐麝香、二甲苯麝香、麝香酮、吐纳麝香和酮麝香6种人造麝香的气相色谱-质谱联用分析方法。方法以面霜、沐浴露、面膜等不同基质的化妆品为试样,选用乙酸乙酯进行提取,固相萃取(solid phase extraction,SPE)小柱净化,采用气相色谱-质谱联用外标法进行分析。结果葵子麝香、佳乐麝香、二甲苯麝香、麝香酮、吐纳麝香和酮麝香6种人造麝香在0.02~0.50μg/mL浓度范围内线性良好,相关系数为0.9968~0.9992。空白样品添加水平分别为0.20、0.40、2.00 mg/kg时,回收率在83.0%~110.38%之间,相对标准偏差在2.8%~7.5%之间,以上6种人造麝香的方法检出下限在20.0~40.0μg/kg之间。结论本方法简单、快速、准确,可满足化妆品中6种人造麝香的同时检测及确证需求。     

杂多酸固相催化合成麝香DDHI的研究

以杂多酸为催化剂 ,2 ,6 二异丙基酚 (DIPP)与异戊二烯 (IP)经环烷基化反应合成麝香DDHI。研究了催化剂种类和用量、原料配比、反应温度及时间对反应结果的影响。反应最佳条件为∶催化剂为磷钨酸固载于活性炭上 ,n(DIPP)∶n(IP) =2 .0 ,m(C1)∶m(IP) =0 .8～ 0 .9,反应温度 36℃～ 4 2℃ ,滴加时间 2h ,保温时间 1h ,产品收率 83.7%。     

Conformational Analysis of Thioether Musks Using Density Functional Theory

A conformational analysis of nine macrocyclic thioether musks has been carried out using molecular mechanics (MMFF), density functional theory (DFT) using both B3LYP and M06 functionals, as well as Hartree-Fock and post-Hartree-Fock (MP2) ab initio methods. 6-Thia-, 10-thia- and 4-methyl-5-thia-14-tetradecananolide, 4-thia-, 7-thia-, 11-thia- and 12-thia-15-pentadecanolide and 6-thia- and 12-thia-16-hexadecanolide were modeled. Unfortunately, there was little agreement between the computational methods at the levels of theory used in this study.     

Analysis of polychlorinated biphenyls, pyrethroid insecticides and fragrances in human milk using a laminar cup liner in the GC injector

 Since 1970 the State Laboratory of Basle City has been periodically analyzing human milk from the region (the latest in 1998/99) as a bioindicator for the environmental load of organochlorine pesticides [1, 2]. The analysis of human milk is very complex including several clean-up steps and is therefore time consuming. The focus is mainly on organochlorine pesticides, polychlorinated biphenyls (PCB), and nitro-musk compounds; analytes which are easily detectable with gas chromatography and electron capture detection (ECD). Our aim was to minimize the clean-up steps for the analysis of ECD sensitive substances. Furthermore, analytes insensitive to EC detection that require MS detection, such as polycyclic musk substitutes, were of interest. With the help of a specially designed GC liner in the vaporizing injector of the gas chromatograph, the laminar cup liner, we have considerably reduced the time and effort in the sample preparation. With the described clean-up procedure we analyzed 53 human milk samples from the region of Basle for PCB, pyrethrins, and pyrethroid insecticides and fragrances (nitro-musk compounds and polycyclic musk substitutes). While PCB showed a general downward trend in mean concentrations since 1980, residues of the polycyclic musk substitutes galaxolide and tonalide were detectable in almost every sample (e.g., 73 μg/kg fat of HHCB, 74 μg/kg fat of AHTN). Pyrethrins and pyrethroid insecticides were detected only at low concentrations between 0.03 and 0.46 mg/kg fat. Received: 28 September 1999 / Revised version: 2 May 2000     

三甲苯麝香合成新工艺的研究

介绍了以炼油厂催化重整的C9重芳烃中的连三甲苯为起始原料经叔丁基化、混酸硝化两步法制备三甲苯麝香的新工艺,实验得出了优化工艺参数。采用高效液相色谱来测定三甲苯麝香的含量,并通过熔点测定、元素分析、核磁共振谱以及红外光谱等手段对三甲苯麝香产品进行了表征。以连三甲苯计三甲苯麝香的总收率达到45％（mol),三甲苯麝香的纯度达到99％以上,连三甲苯两步法合成三甲苯麝香的工艺简单、原料价格便宜、产品收率高,有较好的工业应用前景。     

Preparation of the traditional Chinese medicine compound recipe heart-protecting musk pH-dependent gradient-release pellets

In this study a sustained-release formulation of traditional Chinese medicine compound recipe (TCMCR) was developed by selecting heart-protecting musk pills (HPMP) as the model drug. Heart-protecting musk pellets were prepared with the refined medicinal materials contained in the recipe of HPMP. Two kinds of coated pellets were prepared by using pH-dependent methacrylic acid as film-forming material, which could dissolve under different pH values in accordance with the physiological range of human gastrointestinal tract (GIT). The pellets coated with Eudragit L30D-55, which dissolves at pH value over 5.5, were designed to disintegrate and release drug in the duodenum. The pellets coated with Eudragit L100-Eudragit S100 combinations in the ratio of 1:5, which dissolve at pH value 6.8 or above, were designed to disintegrate and release drug in the jejunum to ileum. The pellets coated with HPMC, which dissolves in water at any pH value, were designed to disintegrate and release drug in the stomach. Finally, the heart-protecting musk sustained-release capsules (HPMSRC) with a pH-dependent gradient-release pattern were prepared by encapsulating the above three kinds of coated pellets at a certain ratio in hard gelatin capsule. The results of dissolution of borneol (one of the active compounds of the TCMCR) in vitro demonstrated that the coating load and the pH value of the dissolution medium had little effect on the release rate of borneol from pellets coated with hydroxypropyl methyl cellulose (HPMC), but had a significant effect on the release rate of borneol from pellets coated with Eudragit L30D-55 or Eudragit L100-Eudragit S100 combinations in the ratio of 1:5. The pellets coated with Eudragit L30D-55 at 30% (w/w) coating load or above had little drug release in 0.1 mol/L HCl for 3 hr and started to release drug at pH value over 5.5. The pellets coated with Eudragit L100-Eudragit S100 combinations in the ratio of 1:5 at 36% (w/w) coating load or higher had little drug release in 0.1 mol/L HCl for 3 hr and in phosphate buffer of pH value 6.6 for 2 hr, and started to release drug at pH value 6.8 or above. The release profiles of lipophilic bornoel and hydrophilic total ginsenoside from HPMSRC, consisting of three kinds of pellets respectively coated at a certain ratio with HPMC, Eudragit L30D-55, and Eudragit L100-Eudragit S100 in the ratio of 1:5, showed a characteristic of pH-dependent gradient release under the simulated gastrointestinal pH conditions and no significant difference between them. The results indicated that various components with extremely different physicochemical properties in the pH-dependent gradient-release delivery system of TCMCR could release synchronously while sustained-releasing. This complies with the organic whole concept of compound compatibility of TCMCR.     

Preparation of the Traditional Chinese Medicine Compound Recipe Heart-Protecting Musk pH-Dependent Gradient-Release Pellets

ABSTRACT

In this study a sustained-release formulation of traditional Chinese medicine compound recipe (TCMCR) was developed by selecting heart-protecting musk pills (HPMP) as the model drug. Heart-protecting musk pellets were prepared with the refined medicinal materials contained in the recipe of HPMP. Two kinds of coated pellets were prepared by using pH-dependent methacrylic acid as film-forming material, which could dissolve under different pH values in accordance with the physiological range of human gastrointestinal tract (GIT). The pellets coated with Eudragit L30D-55, which dissolves at pH value over 5.5, were designed to disintegrate and release drug in the duodenum. The pellets coated with Eudragit L100–Eudragit S100 combinations in the ratio of 1:5, which dissolve at pH value 6.8 or above, were designed to disintegrate and release drug in the jejunum to ileum. The pellets coated with HPMC, which dissolves in water at any pH value, were designed to disintegrate and release drug in the stomach. Finally, the heart-protecting musk sustained-release capsules (HPMSRC) with a pH-dependent gradient-release pattern were prepared by encapsulating the above three kinds of coated pellets at a certain ratio in hard gelatin capsule. The results of dissolution of borneol (one of the active compounds of the TCMCR) in vitro demonstrated that the coating load and the pH value of the dissolution medium had little effect on the release rate of borneol from pellets coated with hydroxypropyl methyl cellulose (HPMC), but had a significant effect on the release rate of borneol from pellets coated with Eudragit L30D-55 or Eudragit L100–Eudragit S100 combinations in the ratio of 1:5. The pellets coated with Eudragit L30D-55 at 30% (w/w) coating load or above had little drug release in 0.1 mol/L HCl for 3 hr and started to release drug at pH value over 5.5. The pellets coated with Eudragit L100–Eudragit S100 combinations in the ratio of 1:5 at 36% (w/w) coating load or higher had little drug release in 0.1 mol/L HCl for 3 hr and in phosphate buffer of pH value 6.6 for 2 hr, and started to release drug at pH value 6.8 or above. The release profiles of lipophilic bornoel and hydrophilic total ginsenoside from HPMSRC, consisting of three kinds of pellets respectively coated at a certain ratio with HPMC, Eudragit L30D-55, and Eudragit L100–Eudragit S100 in the ratio of 1:5, showed a characteristic of pH-dependent gradient release under the simulated gastrointestinal pH conditions and no significant difference between them. The results indicated that various components with extremely different physicochemical properties in the pH-dependent gradient-release delivery system of TCMCR could release synchronously while sustained-releasing. This complies with the organic whole concept of compound compatibility of TCMCR.     

二甲苯麝香和酮麝香的分析方法进展

二甲苯麝香和酮麝香等硝基麝香物质对环境和人体的危害性越来越受到关注,通过介绍二甲苯麝香和酮麝香的理化性质及安全性评价,从样品前处理和检测技术两个方面,综述了不同样品中二甲苯麝香和酮麝香的检测方法,并对各种方法的优缺点进行比较。