正红花油的质量标准研究

目的 建立正红花油中挥发性成分(水杨酸甲酯、丁香油、桂叶油、香茅油)的质量控制标准.方法 采用毛细管气相色谱法对制剂中香叶醇、丁香酚、桂皮醛、水杨酸甲酯、香茅醛和香茅醇进行定性鉴别,并用外标法测定制剂中水杨酸甲酯的含量.结果 香叶醇、丁香酚、桂皮醛、水杨酸甲酯、香茅醛和香茅醇6种成分均达到良好分离,水杨酸甲酯在测定范围...     

气相色谱法测定斑贴膜片中香料混合物含量的研究

目的建立毛细管气相色谱法测定用于检测IV型变态反应的斑贴膜片中7种香料混合物(香叶醇、羟基香茅醛、桂皮醛、丁香酚、戊基桂皮醛、桂皮醇、异丁香酚)含量的方法。方法每片膜片用1 mL乙醇提取30 min,提取液直接注入气相色谱分析,采用极性PEG-20M毛细管气相色谱柱分离,外标法定量。结果 7种香料组份的线性关系良好(r≥0.999 5);精密度和稳定性试验RSD(n=8)均<2%;加标回收率范围95.48%~107.52%,RSD 0.31%~2.00%;贴片香料含量均匀性试验RSD(n=8)<5%;定量限分别为3.7,4.3,3.3,3.5,2.8,2.3,2.9μg.mL 1。结论本方法样品前处理简单,分析快速、准确和灵敏,可满足斑贴膜片中香料混合物定量检测的需要。     

HPLC同时测定补肾活血颗粒中松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛的含量

目的采用HPLC波长切换法,建立同时测定补肾活血颗粒中松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛3成分含量的分析方法。方法采用Zorbax Extend-C18柱(4.6 mm×150 mm,5μm);以乙腈-水为流动相梯度洗脱,松脂醇二葡萄糖苷、苦杏仁苷、桂皮醛的检测波长分别为227,210,290 nm;进行样品前处理工艺和方法学考察。结果松脂醇二葡萄糖苷、苦杏仁苷和桂皮醛均得到很好分离,浓度分别在0.426 0~2.88 6μg·m L?1,7.455~86.60μg·m L?1和0.440 6~13.22μg·m L?1内线性关系良好(r≥0.999);平均加样回收率分别为98.3%(RSD=1.6%),101.4%(RSD=1.1%)和100.0%(RSD=1.2%);精密度试验峰面积RSD均≤1.4%。结论该方法预处理简单,方法灵敏、准确、重复性好,可用于补肾活血颗粒及相关制剂的质量控制。     

纯阳正气胶囊挥发油的质量标准研究

目的 建立纯阳正气胶囊挥发油的质控方法。方法 采用GC法建立挥发油的特征图谱,并测定桂皮醛与丁香酚的含量。结果 15批样品中确定了19个共有峰,指认了峰的归属,选取了9个特征峰建立了特征图谱。桂皮醛与丁香酚分别在0.522～1.565 mg/ml(r=0.999 4)和3.038～9.115 mg/ml(r=0.999 7)范围内线性良好,平均回收率分别为97.1%和97.3%,RSD分别为1.5%、1.4%。结论 所建立的GC特征图谱及含量测定方法可从定性和定量两方面控制纯阳正气胶囊挥发油的质量,方法准确、可行,可作为纯阳正气胶囊挥发油的质量控制方法。     

HPLC测定普力奇降糖胶囊中桂皮醛的含量

目的:建立高效液相色谱法测定普力奇降糖胶囊中桂皮醛含量的方法。方法:采用HPLC法,在波长280nm以乙腈-水-磷酸(42:58:0.2)为流动相,测定桂皮醛的含量。结果:桂皮醛浓度在7.9μg4mL～20.2μg4mL范围内呈良好线性关系(r=0.9992),样品测量稳定性、精密度、重复性良好,平均回收率为98.41%(RSD=0.59%,n=9)。结论:所建立的方法可准确进行定量检测,可用于该制剂的质量控制。     

高效液相色谱法测定丁桂儿脐贴中丁香酚和桂皮醛含量

目的 建立测定丁桂儿脐贴的丁香酚和桂皮醛含量的高效液相色谱法.方法 采用Eclipse XDB-C18色谱柱(150mm×4.6mm,5μm),以甲醇-水(65∶35)为流动相,检测波长280 nm,流速1.0 mL/min.结果 丁香酚进样量在0.172 9～2.074 2 μg范围内与峰面积线性关系良好(r=0.999 9),平均回收率为96.98%,RSD为1.85%(n=6);桂皮醛进样量在0.003 4～0.273 2μg范围内与峰面积线性关系良好(r=0.9999),平均回收率为97.90%,RSD为1.55%(n=6).结论 该方法简便、准确、可靠、精密度高,可用于丁桂儿脐贴的质量控制.     

高效液相色谱法同时测定纯阳正气胶囊中3种成分的含量

目的 采用高效液相色谱法建立同时测定纯阳正气胶囊中橙皮苷、桂皮醛和丁香酚含量的方法。方法 色谱柱为Agilent PorosheⅡ120 EC-C₁₈(4.6 mm×150 mm,4μm),以乙腈-水为流动相梯度洗脱,柱温35℃,流速1.0 ml/min,检测波长284 nm。结果 方法学验证表明,橙皮苷、桂皮醛和丁香酚3种成分线性关系良好(r≥0.999 9),精密度小于2.0%,平均加样回收率在98.0%～101.9%之间,稳定性和重复性的RSD均<3.0%,符合方法学要求。结论 该方法简便、稳定、重复性好、准确可靠,可用于纯阳正气胶囊的质量控制。     

甘桂龙牡浓缩丸质量标准研究

目的建立甘桂龙牡浓缩丸的质量标准。方法采用薄层色谱法对浓缩丸中的甘草、酸枣仁进行定性鉴别;采用高效液相色谱法测定制剂中桂皮醛含量,并对测量方法进行方法学研究。结果甘草、酸枣仁特征斑点清晰,分离度好,阴性对照无干扰。桂皮醛在0.496 8～4.968 0μg范围内呈良好的线性关系,r=0.999 9,平均回收率为99.15%,RSD=0.87%(n=6)。结论所建立的方法简便准确,专属性、重复性好,可作为甘桂龙牡浓缩丸的质量控制标准。     

GC法测定香茅中香叶醇的含量

目的:建立测定香茅中香叶醇含量的方法。方法:采用超声提取法提取香茅中香叶醇,通过气相色谱法测定香叶醇的含量。色谱柱为Agilent Technologies DB-WAX(30m×0.25mm×0.25μm),以聚乙二醇(PEG-20M)为固定相,柱温为130℃,进样口温度为230℃,检测器温度为250℃,氮气(载气)流量为1.0mL.min-1,氢气(燃气)流量为40mL.min-1,空气(助燃气)流量为400mL.min-1。结果:香叶醇进样量在0.0153～0.1071μg范围内与峰面积积分值呈良好线性关系(r=0.9973);平均加样回收率为97.8%,RSD=1.68%(n=6)。结论:本方法简便、快速、准确、重复性好,可用于香茅的质量控制。     

HPLC法测定瑞克卫瑞消毒液中桂皮醛和丁香酚的含量

目的建立测定瑞克卫瑞消毒液中桂皮醛和丁香酚含量的高效液相色谱方法。方法色谱柱:采用Welchrom C18柱(250mm×4.6mm,5μm);流动相:甲醇-水(60∶40);流速:1.0mL.min-1;柱温:25℃;检测波长:280nm。结果桂皮醛在0.21～2.1μg(r2=0.999 1)范围内线性关系良好,平均加样回收率为101.3%,RSD为0.1%;丁香酚在0.42～4.2μg(r2=0.999 9)范围内线性关系良好,平均加样回收率为96.7%,RSD为0.3%。结论该方法简单、快速、重复性好,可用于瑞克卫瑞消毒液的质量控制。     

Plasma salicylate from methyl salicylate cream compared to oil of wintergreen

BACKGROUND: Poison Control Centers follow the acetylsalicylic acid (ASA) treatment guideline to manage unintentional ingestions of topical methyl salicylate liniments. For example, one teaspoon of 30% methyl salicylate cream such as Ben Gay provides an "ASA equivalent dose" of 180 mg/kg for a 10 kg child. The ASA treatment guideline advises emesis with syrup of Ipecac and 24 h home followup for this dose. Both the ASA conversion factor to yield the ASA equivalent dose and the treatment guideline assume 100% bioavailability of the salicylate. The nature of this topical dosage product led the investigators to expect less than complete absorption of methyl salicylate. OBJECTIVE: To compare plasma concentrations of salicylate from ingested methyl salicylate cream with plasma concentrations of salicylate from ingested oil of wintergreen. METHODS: Four adult volunteers consented to an open label, four-way crossover design, with randomization to the following treatments: 1 mL Oil of Wintergreen, U.S.P., 6.7 g of Ben Gay 15% and 20 g of Ben Gay 15% and also to hold 5 g of Ben Gay 15% cream in the buccal cavity for 1 minute and then expectorate. Plasma was collected for salicylate determination, and the results analyzed with a noncompartmental pharmacokinetic model. RESULTS: No plasma salicylate was detected after buccal treatment phase. Relative bioavailability for the low-dose treatment was 0.5 compared to oil of wintergreen. CONCLUSION: Plasma salicylate concentrations from methyl salicylate cream are not equal to those achieved after ingestion of oil of wintergreen. Dosage formulation must be considered when predicting toxicity.     

GC/FTIR联用分析麝香风湿油

本文用气相色谱/富里叶变换红外光谱联用对中成药麝香风湿油作了分析研究,鉴定了其中的十个主要组分。并对其中三个组分用气相色谱内标法做了含量测定。平均回收率为100±1.0%,变异系数<2.0%。     

Sedative effects of vapor inhalation of the essential oil of <Emphasis Type="Italic">Microtoena patchoulii</Emphasis> and its related compounds

Microtoena patchoulii (Labiatae) is a perennial herb that grows in southern China. In the present study, the sedative activity of the essential oil of the leaves was evaluated using mice when the volatile oil was administered by inhalation. The inhalation of the oil by mice significantly reduced the spontaneous motor activity. Fractionation of the oil revealed that the main constituents in the oil were 1-octen-3-ol, terpinolene, patchouli alcohol, and methyl salicylate. Each 1-octen-3-ol, terpinolene, or patchouli alcohol significantly reduce the locomotor activity when it was administered singly. However, the essential oil fraction containing both patchouli alcohol and methyl salicylate did not exhibit any effects. It is suggested that methyl salicylate might negate the sedative effect of patchouli alcohol, and that the concentration ratios of the compounds in vapor would play important roles as sedatives. In order to clarify the mechanism of action, the effects of these compounds on caffeine-induced excitation and pentobarbital-induced elongation of sleeping time in mice were tested. Each 1-octen-3-ol or terpinolene reduced the locomotor activity excited by caffeine to those of normal levels. Elongation of sleeping time induced by pentobarbital was further elongated by the inhalation of terpinolene, but not by that of 1-octen-3-ol. It is indicated that terpinolene is a potent suppressor of the central nervous system.     

Rheological and drug release properties of oil gels containing colloidal silicon dioxide.

The rheological properties of oil gels prepared by dispersing colloidal silica in n-dodecane and 1-dodecanol were examined. The differences in gel strength using these two media were accounted for by the difference in the extent of hydrogen bond formation between the silanol groups on the silica surface. The incorporation of methyl salicylate further modified the rheological properties of the gels. The drug was capable of hydrogen bonding with silanol groups in the n-dodecane gels, which increase gel strength at low concentrations; at high concentrations, the drug acted as a plasticizer. In 1-dodecanol systems, the drug acted solely as a plasticizer. Adsorption studies showed that methyl salicylate was adsorbed only on the silica particles in the n-dodecane medium. Interaction of the drug with the silanol groups in the n-dodecane systems did not appear to effect methyl salicylate release from the gels.     

Fourier transform mid-infrared (MIR) and near-infrared (NIR) spectroscopy for rapid quality assessment of Chinese medicine preparation Honghua Oil

Honghua Oil (HHO), a traditional Chinese medicine (TCM) oil preparation, is a mixture of several plant essential oils. In this text, the extended ranges of Fourier transform mid-infrared (FT-MIR) and near infrared (FT-NIR) were recorded for 48 commercially available HHOs of different batches from nine manufacturers. The qualitative and quantitative analysis of three marker components, alpha-pinene, methyl salicylate and eugenol, in different HHO products were performed rapidly by the two vibrational spectroscopic methods, i.e. MIR with horizontal attenuated total reflection (HATR) accessory and NIR with direct sampling technique, followed by partial least squares (PLS) regression treatment of the set of spectra obtained. The results indicated that it was successful to identify alpha-pinene, methyl salicylate and eugenol in all of the samples by simple inspection of the MIR-HATR spectra. Both PLS models established with MIR-HATR and NIR spectral data using gas chromatography (GC) peak areas as calibration reference showed a good linear correlation for each of all three target substances in HHO samples. The above spectroscopic techniques may be the promising methods for the rapid quality assessment/quality control (QA/QC) of TCM oil preparations.     

大圣油中薄荷脑与水杨酸甲酯的气相色谱法测定

本文采用气相色谱法测定大圣油中薄荷脑、水杨酸甲酯的含量。     

Hydrogel-thickened nanoemulsion system for topical delivery of lipophilic drugs

In this work, a hydrogel-thickened nanoemulsion system (HTN) with powerful permeation ability, good stability and suitable viscosity was investigated for topical delivery of active molecules. HTN was prepared to deliver an oily mixture of 5% camphor, 5% menthol and 5% methyl salicylate for topical therapy of arthritis, minor joint and muscle pain using soybean oil as the oil phase, soybean lecithin, Tween 80 and poloxamer 407 as the surfactants, propylene glycol as the cosurfactant, carbomer 940 as a thickening agent. The HTN system was found to combine the o/w microstructure of nanoemulsion with the gel network of hydrogel and had a suitable viscosity of 133.2PaS. The system had small average diameters and good long-term stability. The abilities of HTN to deliver the high amounts of camphor, menthol and methyl salicylate were evaluated using the in vitro permeation studies. The permeation rates of camphor, menthol and methyl salicylate from the optimal HTN formulation were 138.0+/-6.5, 63.6+/-3.3, 53.8+/-3.2 microg cm(-2) h(-1) and showed the significant advantages over the control gel. The HTN with good stability and powerful permeation enhancing ability and suitable viscosity might be a promising prospective carrier for topical delivery of lipophilic drugs.     

A critical review of the literature to conduct a toxicity assessment for oral exposure to methyl salicylate

Methyl salicylate is the predominant constituent of oil of wintergreen and is used as a pesticide, a denaturant, an external analgesic, a fragrance ingredient, and a flavoring agent in products such as chewing gum, baked goods, syrups, candy, beverages, ice cream, and tobacco products; and it occurs naturally in some vegetables and berries. Methyl salicylate is of interest to the tobacco industry as oil of wintergreen is used as a flavorant in tobacco products. The purpose of this investigation was to conduct a critical review of the available literature for oral exposure to methyl salicylate, incorporating an analysis of the quality of the studies available and the current understanding of the mode of action. Following a review of all of the available literature, the most appropriate data sets for dose-response modeling were reported by Gulati et al. in which significant changes in reproductive/development endpoints were reported to occur after exposure to 500?mg/kg/d of methyl salicylate in male and female mice. Benchmark dose modeling was performed and the most sensitive endpoint, the number of litters per mating pair, was associated with a BMDL of 220?mg/kg/d. This BMDL was chosen as the point of departure and adjusted by a body weight scaling factor to derive a human equivalent dose. Based on the uncertainty factor analysis, the POD for methyl salicylate was adjusted by a UF of 3 for interspecies uncertainty to derive an allowable daily intake of 11?mg/kg/d.     

The analysis of methyl salicylate and salicylic acid from Chinese herbal medicine ingestion

This paper presents a multi-drug fatality in which methyl salicylate was ingested. It is presented to inform the toxicological community that a particularly expeditious method of detection for methyl salicylate exists. Previously published methods for the analysis of methyl salicylate include a gas chromatographic-mass spectrometric method and an alkaline/acidic extraction followed by high-performance liquid chromatographic (HPLC) analysis. This article describes a method for analyzing methyl salicylate using HPLC, in which a simple, rapid extraction procedure is used. Using a previously published HPLC method, methyl salicylate and salicylic acid were easily identified in biological specimens. Methyl salicylate and salicylic acid were detected using an extraction solution of acetonitrile coupled with internal standard and then analyzed by HPLC-diode-array detection. Because of its concentrated liquid form, methyl salicylate ingestion can cause rapid onset salicylate toxicity. As the potentially fatal methyl salicylate forms are readily available and easily found on drugstore shelves, the need to rapidly detect and quantitate salicylic acid concentrations that are due to methyl salicylate ingestion may arise. In the case presented, the peripheral blood concentration of salicylic acid from methyl salicylate ingestion was 320 mg/L, and the concentration in gastric contents was 820 mg. It alone was not the cause of death, however. The discovery of the ability to detect and quantitate methyl salicylate was due to its suspected ingestion.     

水杨酸甲酯六角相液晶的处方筛选与体外透皮研究

目的 优选出水杨酸甲酯六角相液晶的最优处方,并考察所制备的水杨酸甲酯六角相液晶的体外透皮性能.方法 以植烷三醇为基质,采用自乳化法制备水杨酸甲酯六角相液晶;以累积渗透量为指标,采用单因素考察法优化处方;通过偏光显微镜和小角度X射线散射仪对制备的水杨酸甲酯六角相液晶进行表征;并采用改良Franz扩散池考察水杨酸甲酯六角相液晶的透皮性能.结果 水杨酸甲酯六角相液晶最佳处方为植烷三醇66%,水22%,水杨酸甲酯12%;所制得的水杨酸甲酯六角相液晶为六角相;体外透皮实验显示,水杨酸甲酯六角相液晶的累积渗透量是市售复方水杨酸甲酯软膏的2.76倍.结论 优选的水杨酸甲酯六角相液晶可显著提高水杨酸甲酯的透皮性能,为水杨酸甲酯六角相液晶的进一步研究提供参考依据.