高效液相色谱法同时测定麻黄-桂枝药对中7种成分含量

目的 建立同时测定麻黄-桂枝药对中盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱、桂皮酸、桂皮醇、桂皮醛、香豆素7种成分含量的高效液相色谱法.方法 色谱柱为Agilent Zorbax Eclipse Plus C18柱(250 mm×4.6 mm,5μm),流动相为乙腈-含0.1％NH4Cl的0.05％磷酸水溶液(梯度洗脱...     

配伍对麻黄甘草药对中麻黄类生物碱在大鼠体内组织分布的影响

目的：研究麻黄与甘草配伍前后麻黄类生物碱在 SD 大鼠组织分布特点,从药物相互作用角度揭示甘草对麻黄类生物碱组织分布的影响。方法采用超高效液相色谱-串联质谱（ UPLC - MS/ MS）法在多反应监测（MRM）模式下测定麻黄与甘草配伍前后不同时间点大鼠各组织液中麻黄类生物碱的浓度,比较麻黄与甘草配伍前后麻黄类生物碱组织分布的差异。结果与麻黄组相比,麻黄与甘草配伍后,促进了去甲基麻黄碱、麻黄碱和伪麻黄碱在研究组织中的吸收和分布;加快了去甲基麻黄碱、麻黄碱、伪麻黄碱和甲基麻黄碱从脑组织中消除;抑制了去甲基伪麻黄碱在心和脑组织中的吸收和分布,并加快了其从心和脑组织中的消除;不同程度地加快了去甲基麻黄碱从心、肺、肾的消除,加快了麻黄碱从心组织中消除,加快了甲基麻黄碱从肺和肾中的消除。结论麻黄与甘草配伍对麻黄类生物碱在大鼠组织中的分布具有显著的影响。     

麻黄、含麻黄中成药及生物体液中麻黄碱的定量分析方法

麻黄是一种常用中药 ,为麻黄科多年生草本状小灌木草麻黄 (ＥｐｈｅｄｒａｓｉｎｉｃａＳｔａｐｆ.)或木贼麻黄(Ｅ .ｅｑｕｉｓｅｔｉｎａＢｕｎｇｅ .)和中麻黄 (Ｅ .ｉｎｔｅｒｍｅｄｉａＳｃｈｒｅｎｋｅｔＭｅｙ .)的草质茎 ,是提取麻黄碱和制成多种制剂的原料。麻黄含生物碱 10种以上 ,主要是 3对立体异构的生物碱 ,即 :左旋麻黄碱 (ｌ -ｅｐｈｅｄｒｉｎｅ) ,右旋伪麻黄碱 (ｄ -ｐｓｅｕｄｏｅｐｈｅｄｒｉｎｅ) ;左旋去甲基麻黄碱 (ｌ-ｎｏｒｅｐｈｅｄｒｉｎｅ) ,右旋去甲基伪麻黄碱 (ｄ -ｎｏｒｐｓｅｕｄｏｅｐｈｅｄｒｉｎｅ) ;…     

LC-MS/MS法测定麻黄-桂枝药对中11个成分及其溶出影响的探讨

目的 建立麻黄-桂枝药对中原儿茶酸、儿茶素、表儿茶素、丁香醛、香豆素、肉桂醇、肉桂酸、桂皮醛、麻黄碱、伪麻黄碱和甲基麻黄碱11个成分的LC-MS/MS含量测定方法,并探讨单煎共煎对11个成分溶出的影响。方法 分别以麻黄桂枝共煎液、单煎液、单煎合并液为样品,采用高效液相色谱-串联质谱（LC-MS/MS）法测定8个苯丙素类成分和3个麻黄类生物碱的含量。结果 11个成分在各自范围内均呈良好的线性关系（r≥0.994 8）;平均加样回收率为98.30%～100.92%,RSD≤5.85%（n=9）;精密度、重复性和稳定性均良好,符合方法学考察要求。麻黄与桂枝共煎时,8个苯丙素类成分煎出量均有不同程度的降低,而3个麻黄类生物碱均有不同程度升高。结论 该方法简便快速、准确可靠,可用于11个成分的含量测定,共煎对麻黄桂枝各自成分的溶出均具有一定的影响。     

麻黄中麻黄生物碱的气相色谱测定法

本文应用毛细管气相色谱法,配备氮磷检测器对麻黄中六种生物碱:麻黄碱、伪麻黄碱、去甲麻黄碱、去甲伪麻黄碱、甲基麻黄碱和甲基伪麻黄碱进行分离、测定。对生药样品预处理方法作了较大改进,采用直接碱化醚提法。简化操作步骤。用内标法,线性方程定最测定了国产十二种麻黄,结果与高效液相色谱法基本一致。     

十二种国产麻黄的品质评价

本文应用高效液相色谱法对我国24个产地所产的12种麻黄生药进行了六种生物碱的定量分析,这六种生物碱是:麻黄碱(ephedrine),伪麻黄碱(pseudoephedrine),去甲基麻黄碱(norephedrine),去甲基伪麻黄碱(norpseudoephedrine),甲基麻黄碱(methylephedrine)和甲基伪麻黄碱(methylpseudoephedrine)。根据分析结果,对这些麻黄生药的品质作出了评价。     

微透析法研究麻黄汤对大鼠脑海马区氨基酸类神经递质释放的影响

目的应用微透析技术,研究中医经典方剂——麻黄汤对大鼠脑海马区4种氨基酸类神经递质(谷氨酸Glu、甘氨酸Gly、天冬氨酸Asp、γ-氨基丁酸GABA)释放的影响,并与麻黄药材、麻黄生物碱的作用相对比。方法 SD大鼠分为6组:麻黄汤高剂量组(以麻黄生药计4 g·kg~(-1))、中剂量组(以麻黄生药计2 g·kg~(-1))、低剂量组(以麻黄生药计1 g·kg~(-1))、麻黄药材组(以麻黄生药计2 g·kg~(-1))、麻黄生物碱组(麻黄碱7 mg·kg~(-1)、伪麻黄碱2.4 mg·kg~(-1)、甲基麻黄碱1.12 mg·kg~(-1))以及空白对照组。在动物清醒状态下,微透析采样技术从大鼠脑海马区取样,建立邻苯二甲醛柱前衍生高效液相色谱-电化学法(HPLC-ECD)检测脑透析液中4种神经递质的含量。结果 4种氨基酸类神经递质在28 min内达到良好的分离。麻黄汤各剂量组、麻黄药材组和麻黄生物碱组大鼠脑海马区4种神经递质的含量均增加,与空白对照组比较差异有显著性(P<0.05)。与中剂量麻黄汤组比较,麻黄生物碱组在90 min时明显降低了抑制性氨基酸神经递质Gly和GABA水平。大鼠口服麻黄汤各剂量、麻黄药材水煎液后,海马区兴奋性神经递质Asp和Glu水平呈先增后降的趋势,麻黄汤各剂量组大鼠Glu和Asp水平在给药后90~120 min达峰值,随着麻黄汤给药剂量的增加,Asp和Glu含量亦增加。与中剂量麻黄汤组比较,麻黄水煎液组和麻黄生物碱组Glu水平分别在90 min和150 min达峰值,达峰值时Glu含量均明显增加。结论麻黄汤剂量与Asp、Glu含量的增加呈现一定的正相关性。麻黄汤中其它组分抑制了麻黄和麻黄生物碱升高Glu水平的作用,同时促进了麻黄生物碱对GABA及Gly含量的升高作用。     

HPLC测定麻黄及其制剂中3种生物碱含量

目的 建立HPLC同时测定麻黄及其制剂中3种生物碱含量。方法 以乙腈-甲醇-0.1%磷酸溶液(1.5∶4∶94.5)为流动相,同时测定麻黄、金麻杏止咳片和麻杏止咳片中3种生物碱的含量。结果 盐酸麻黄碱、盐酸伪麻黄碱、盐酸甲基麻黄碱的进样量分别为0.102 9~0.686,0.025?11~0.167 4,0.022 23~0.148 2 μg,分别与峰面积呈良好的线性关系;平均回收率分别为100.56%,97.84%和98.42%,RSD分别为0.20%、0.94%和1.31%(n=6)。结论 所建立的HPLC可通过测定3种生物碱的含量综合评价麻黄及其制剂的质量。     

气相色谱-质谱和化学计量学解析法分析药对麻黄-桂枝挥发油成分

利用气相色谱-质谱对药对麻黄-桂枝及单味药麻黄和桂枝的挥发油成分进行检测，通过化学计量学解析法对产生的二维色谱-质谱数据进行解析，得到各组分的纯色谱和质谱，根据其保留时间和质谱，在质谱库中进行相似检索，实现对组分的定性，再用总体积积分法进行定量。麻黄-桂枝、麻黄和桂枝挥发油分别定性了97，72和68个色谱峰，占总含量的89.76%，90.08%和91.62%。药对挥发油成分的数目大致为麻黄和桂枝挥发油成分的加和，但相对含量有变化。     

不同地区市售麻黄药材中盐酸麻黄碱、盐酸伪麻黄碱和总生物碱的含量测定

目的:对全国不同地区市售麻黄药材中盐酸麻黄碱、盐酸伪麻黄碱和总生物碱的含量进行测定,从化学成分的角度对其质量进行评估。方法:收集了28个批次来源于全国7个不同产地、21个不同地区的麻黄药材,按照2010版《中国药典》的方法测定其中盐酸麻黄碱、盐酸伪麻黄碱的含量;建立酸性染料比色法测定药材中的总生物碱。结果:有10个批次的麻黄药材(占全部批次的35.7%)达不到2010版《中国药典》的要求(盐酸麻黄碱和盐酸伪麻黄碱的总质量分数不得少于0.80%),且28个批次的样品中两种生物碱的总质量分数最高与最低相差45倍,总生物碱的质量分数最高与最低相差33倍。结论:所建立的酸性染料比色法测定麻黄总生物碱的含量方法简便、重复性好。市售麻黄药材以草麻黄为主,有效成分生物碱的含量差异较大,劣质情况较为严重。有必要加强麻黄药材的市场监管,保证其临床应用的安全、有效。     

HPLC法同时测定小建中汤中肉桂酸和桂皮醛的含量

目的建立高效液相色谱法同时测定小建中汤中肉桂酸及桂皮醛的含量。方法高效液相色谱法,色谱柱:Phenomenex ODS3柱(4.6 mm×250 mm,5μm);流动相:乙腈-0.1%的磷酸水溶液(35∶65);流速:1.0 mL·min-1;柱温:30℃;检测波长:280 nm。结果肉桂酸与桂皮醛分别在2.0～50.0μg·mL-1与2.0～25.0μg·mL-1浓度范围内呈良好线性关系;平均回收率为99.8%与101.0%。结论本方法可更加全面地控制制剂质量。     

Antiradical activity of cinnamic acid derivatives

The antiradical activity (ARA) of cinnamic acid derivatives and their structural analogs was evaluated by the ability to inhibit chemiluminescence in a system generating free radicals. The results showed that the ARA of the studied compounds is characterized by the same features as those established previously for the antioxidant activity of these compounds.     

Human skin absorption and metabolism of the contact allergens, cinnamic aldehyde, and cinnamic alcohol

trans-Cinnamaldehyde and trans-cinnamic alcohol have been commonly reported to cause allergic contact dermatitis (ACD) in humans. Cinnamaldehyde is a more potent skin sensitizer than cinnamic alcohol. It has been hypothesized that cinnamic alcohol is a "prohapten" that requires metabolic activation, presumably by oxidoreductase enzymes such as alcohol dehydrogenase (ADH) or cytochrome P450 2E1 (CYP2E1), to the protein-reactive cinnamaldehyde (a hapten). In this study, the in vitro percutaneous absorption and metabolism of cinnamaldehyde and cinnamic alcohol (78 micromol dose) has been examined using freshly excised, metabolically viable, full-thickness breast and abdomen skin from six female donors. Penetration rates and total cumulative recoveries of cinnamic compounds that were present in receptor fluid, extracted from within the skin, evaporated from the skin surface, or remained unabsorbed on the skin surface after 24 h were quantified by reversed-phase high-performance liquid chromatography. Biotransformation of cinnamaldehyde to both cinnamic alcohol and cinnamic acid was observed. Topically applied cinnamic alcohol was converted to cinnamaldehyde (found on the skin surface only) and cinnamic acid. To establish whether these biotransformations were enzymatic, experiments were performed in the absence and presence of varying concentrations (80-320 micromol) of the ADH/CYP2E1 inhibitors pyrazole or 4-methylpyrazole. The observation that pyrazole significantly reduced (p < 0.05) the total penetration of cinnamic metabolites into receptor fluid, following either cinnamaldehyde or cinnamic alcohol treatment, but did not significantly affect parent chemical penetration, suggests that we are measuring cutaneous metabolic products of ADH activity. The skin absorption and metabolism of cinnamaldehyde and cinnamic alcohol will play an important role in the manifestation of ACD following topical exposure to these compounds.     

Hepatoprotective activity of analogs of cinnamic acid

The hepatoprotective activity of 16 derivatives of +hydroxycinnamic acids was studied on the model of acute tetrachloromethane-induced hepatitis. The effects of the agents administered in doses of 5, 15, and 30 mg/kg were compared with those of silibor, vitamin E and flamine. The studied compounds were shown to possess the bile-expelling, antioxidant and membrane-protective effects being superior in some cases to similar effects of reference drugs. The structure-activity relationship was established.     

Tyrosinase inhibitory activities of cinnamic acid analogues

The aim of this study was to show how tyrosinase inhibitory activity is correlated with the structure of cinnamic acid derivatives. We synthesized cinnamic acid derivatives, and investigated their tyrosinase inhibitory and DPPH radical scavenging activities. The results show that reduction of C=C double bonds and the substituent group of cinnamic acid derivatives have an effect on antioxidant activity and tyrosinase inhibitory activity. Among these compounds, compounds 2, 6 and 6a showed a potent tyrosinase inhibitory activity with IC50 (50% inhibitory concentration) values of 115.6 microM, 114.9 microM and 195.7 microM, respectively. The results obtained provide a useful clue for the design and development of new tyrosinase inhibitors.     

Antioxidant and antimicrobial activities of cinnamic acid derivatives

Cinnamic acid is an organic acid occurring naturally in plants that has low toxicity and a broad spectrum of biological activities. In the search for novel pharmacologically active compounds, cinnamic acid derivatives are important and promising compounds with high potential for development into drugs. Many cinnamic acid derivatives, especially those with the phenolic hydroxyl group, are well-known antioxidants and are supposed to have several health benefits due to their strong free radical scavenging properties. It is also well known that cinnamic acid has antimicrobial activity. Cinnamic acid derivatives, both isolated from plant material and synthesized, have been reported to have antibacterial, antiviral and antifungal properties. Acids, esters, amides, hydrazides and related derivatives of cinnamic acid with such activities are here reviewed.     

Fragrance material review on cinnamic acid.

A toxicologic and dermatologic review of cinnamic acid when used as a fragrance ingredient is presented.     

Cytotoxicity of cinnamic aldehyde on leukemia L1210 cells

Cytotoxic effect of cinnamic aldehyde (CA) on L1210 mouse leukemia cells was tested. Addition of CA in Fischer's medium at 4.8 micrograms/ml could inhibit the growth of L1210 by 50 per cent. The terminal aldehyde-group of CA molecule was found to be responsible to the inhibition. Experiments of incorporating [3H]-uridine, [3H]-thymidine, and [3H]-leucine by the cells revealed that the syntheses of protein, DNA, and RNA were suppressed by the presence of CA in the culture solution with potency appeared in that order. The inhibitory effect of CA on glycolysis was insignificant. Direct reaction between aldehyde-groups of CA molecules and sulfhydryl-groups of cell components was proved. The results suggested that CA inhibited L1210 cells by blocking protein synthesis through trapping sulfhydryl-containing amino acids in the cell.