不同品种陈皮中辛弗林的含量分析

目的 建立陈皮中辛弗林简单快速的测定方法,对5种不同品种陈皮中的辛弗林进行含量分析.方法 利用单因素考察法考察最佳提取条件,采用薄层-紫外法分离测定陈皮中的辛弗林.结果 辛弗林在10～60 μg/ml(R2=0.9996,n=6)范围内浓度与吸光度呈良好的线性关系.不同品种陈皮中辛弗林的含量存在差异,含量在11.71 ～13.84 mg/g之间,其中脐橙皮中辛弗林含量最高.结论 该法测定陈皮中辛弗林含量,重复性较好,对仪器要求不高,准确可靠,可用于陈皮质量控制.     

广陈皮和青皮炮制前后辛弗林含量比较研究

目的:分析广陈皮、青皮炮制前后辛弗林的含量变化,为探讨炮制原理提供试验依据.方法:以微波光波法提取炮制前后广陈皮、青皮饮片中的辛弗林,采用HPLC法对所提取辛弗林的含量进行测定.结果:广陈皮和青皮中辛弗林含量分别在0.42%和0.45%左右,经炮制以后辛弗林的含量变为0.49%和0.36%左右.结论:广陈皮和青皮炮制前...     

高效液相色谱法测定青皮中辛弗林和N-甲基酪胺的含量

目的 :建立青皮中辛弗林和N 甲基酪胺的含量测定方法。方法 :样品用 30 %甲醇超声提取 30min。ODS柱 ,甲醇-水-十二烷基硫酸钠 (5 5∶4 5∶0 .1)为流动相 ,检测波长 275nm。结果 :辛弗林和N 甲基酪胺获良好分离 ,辛弗林在 0 .35 μg～ 11.2 4 μg线性关系良好 (r=0 .9999) ,加样回收率为 97.1% ,重现性为 1.9%。 结论 :该方法可用于青皮的质量控制。     

正交试验优选枳实中辛弗林提取工艺

目的:研究枳实中辛弗林的最佳提取工艺。方法:以辛弗林的转移率为指标,考察了不同提取溶剂和提取方式对辛弗林提取率的影响,在此基础上采用正交试验设计,考察了加水量、煎煮温度、煎煮时间3个因素对辛弗林提取率的影响。结果:加水回流提取辛弗林的提取率较高,确定枳实的最佳提取工艺为:回流提取3次,提取1 h,加水依次为12,10,10倍量。结论:工艺条件简单,稳定,可行,辛弗林提取率高,为改进枳实的提取工艺提供了依据。     

玳玳黄酮降脂提取物的鉴别及其特殊杂质检测

目的:建立玳玳黄酮降脂提取物的鉴别及其特殊杂质辛弗林的检测方法。方法:采用薄层色谱法(TLC)鉴别玳玳黄酮降脂提取物,检测玳玳黄酮降脂提取物中可能存在的特殊杂质辛弗林。结果:以氯仿:甲醇:水(13∶6∶2)下层溶液为展开剂,玳玳黄酮降脂提取物中主成分得到快速、有效地分离鉴别;以正丁醇:乙酸乙酯:氨水:水(9∶3∶1∶2)为展开剂,检测辛弗林方法灵敏度高,斑点显色清晰,易于观察,最低检测限是0.08μg,玳玳黄酮降脂提取物中辛弗林的含量均小于10×10-6。结论:本实验所建立的方法能有效用于玳玳黄酮降脂提取物的鉴别与特殊杂质辛弗林的检查。     

树脂分离纯化枳实中辛弗林的工艺研究

目的 研究大孔吸附树脂对枳实中辛弗林的吸附性能,考察精制工艺.方法 以辛弗林质量分数和收率为考察指标,比较了HPD.300、NKA.9、AB.8、D001-cc 等树脂对枳实中辛弗林的吸附和解吸特性,以及纯化能力.结果 D001-cc 树脂具有最佳的吸附洗脱参数,上样液生药质量浓度为0.5 g生药/mL,4倍体积蒸馏水、2倍体积1.5 mo1/L氨水依次洗脱,产物中辛弗林质量分数为46.3%.得率为1%.结论 D001.cc树脂对枳实中辛弗林综合性能较好,适合于辛弗林的分离精制.     

心脉康片的提取工艺优选

目的:优选心脉康片的提取工艺.方法:采用热循环回流提取浓缩机组方法,以干膏得率和辛弗林含量为指标,HPLC测定辛弗林含量,采用L9(34)正交试验对影响提取工艺的提取时间、加水量和蒸汽压进行考察.结果:心脉康片的最佳提取工艺为加15倍量水循环回流提取4h,蒸汽压0.15 MPa.结论:该优选的提取工艺稳定、合理,可作为心脉康片的工业化生产提取工艺.     

枳实、枳壳、青皮和陈皮等药材中辛弗林含量测定研究

西方食品增补剂禁用麻黄后化学结构与麻黄碱相似的辛弗林（synephrine）又备受关注。本文从含量测定的角度,建立了辛弗林含量测定方法。分析了枳实、枳壳、青皮和陈皮药材共95份样品中辛弗林的含量分布情况,并采用该方法考察了新会、长沙和自贡产地自采果皮在不同采收时间内辛弗林含量变化情况。测定结果表明,青皮和枳实药材中辛弗林含量最高,约为0．6％和0．45％,陈皮和枳壳中相对略少,为0．3％和0．1％;未成熟药材（青皮）辛弗林含量比成熟果皮为高。由此推算相应的用药剂量,从而为检测和使用枳实、枳壳、青皮和陈皮等药材提供参考和依据.     

中药枳实中辛弗林存在状态与其纳滤传质过程的相关性

该文基于纳滤分离中的溶解-扩散效应和电荷效应理论,拟合传质系数与初始浓度的相关性,构建预测辛弗林传质过程中的数学模型,并验证其适用性。实验结果表明,操作压力与膜通量存在线性关系,随着辛弗林浓度升高膜通量出现衰减。在溶解-扩散效应和电荷效应的双重作用下,其传质系数与初始浓度呈现幂函数相关,回归系数均大于0.9,发现解离状态下的辛弗林传质系数小于游离态及解离-游离共存态。建立的纳滤传质预测数学模型,通过枳实提取液验证发现辛弗林截留率与实验值接近,该模型实用可行。以辛弗林为例建立的纳滤分离预测模型,解决了中药生物碱类成分纳滤分离机制不清晰的问题,为中药生物碱类成分的常温化精制富集提供理论和技术支撑。     

同一植株不同生长期橘皮中辛弗林含量动态变化规律研究

目的:比较研究定产地、定植株橘皮在不同生长期橘皮中辛弗林的动态变化差异,探索橘皮因采收期不同而成为(陈皮和青皮)2味功效存在差异的中药其内在物质基础有何不同,以及采收期与有效成分的动态累积的关系,为两药质量控制标准的完善提供依据.方法:采用HPLC测定四川蒲江、眉山、夹江及重庆市璧山4个不同产地、不同采收期共45批橘皮中的辛弗林含量.结果:同一植株不同生长期橘皮中辛弗林含量随着果实成熟度增加而降低,11月之后采集的样品辛弗林的含量变化趋于稳定;同一植株不同年份相同生长期的橘皮药材中辛弗林含量亦无显著差异.结论:同一植株不同的采收期对陈皮、青皮辛弗林成分的影响较大,橘皮未成熟的果实中辛弗林的含量最高,不同生长期橘皮辛弗林含量呈随着果实成熟度增加而降低.     

芸香橘科柑属生物碱类成分质量研究

利用反相高效液相色谱定量法进行10种芸香科柑橘属生药生物碱类成分辛弗林的进行了质量标准研究。采用phenomsil C18(250mm×4.6mm,5u)色谱柱,辛弗林其流动相采用甲醇一水(7∶4)(水中含0.02%磷酸和0.1%十二烷基硫酸钠)。其中辛弗林在1.1320～14.152μg.μL-1,线性关系良好(r=0.997);加样回收率分别为98.0%。测定结果显示不同原植物和产地来源的各橘属生药中辛弗林的含量差别较大。且随着果实成熟程度的增加,辛弗林有下降的趋势;而整个果实辛弗林含量大于某一部分,为药材的标准化研究提供科学的方法和试验依据。     

枳实、枳壳、青皮和陈皮等药材中辛弗林含量测定研究

西方食品增补剂禁用麻黄后化学结构与麻黄碱相似的辛弗林（synephrine）又备受关注。本文从含量测定的角度，建立了辛弗林含量测定方法。分析了枳实、枳壳、青皮和陈皮药材共95份样品中辛弗林的含量分布情况，并采用该方法考察了新会、长沙和自贡产地自采果皮在不同采收时间内辛弗林含量变化情况。测定结果表明，青皮和枳实药材中辛弗林含量最高，约为0．6％和0．45％，陈皮和枳壳中相对略少，为0.3％和0．1％；未成熟药材（青皮）辛弗林含量比成熟果皮为高。由此推算相应的用药剂量，从而为检测和使用枳实、枳壳、青皮和陈皮等药材提供参考和依据。     

四磨汤口服液HPLC指纹图谱及其辛弗林、柚皮苷归属分析

目的:建立四磨汤口服液HPLC指纹图谱,明确辛弗林与柚皮苷在图谱中的归属。方法:采用HPLC法,建立四磨汤口服液自制样品在283 nm检测波长下的指纹图谱,以色谱峰保留时间为考察指标,应用辛弗林、柚皮苷对照品及枳壳中药对照药材,对四磨汤口服液HPLC图谱特征峰进行标定,从而获取辛弗林和柚皮苷的归属信息。结果:建立了四磨汤口服液自制样品HPLC特征指纹图谱,标示出8个共有峰,且5个是明显特征峰,各峰分离良好,其中2个明显特征峰的保留时间均与辛弗林、柚皮苷色谱吻合,也与枳壳色谱中的2个特征峰吻合。结论:该方法简便、重现性好,既有利于制定四磨汤口服液质量控制方法,也为深入四磨汤口服液药效物质基础研究和新药研发提供参考。     

不同产地枳壳药材HPLC指纹图谱及其柚皮苷、新橙皮苷和辛弗林含量分析

 目的 研究枳壳药材的HPLC指纹图谱及测定其柚皮苷、新橙皮苷和辛弗林3种成分的含量,以建立药材有效的质量评价方法。方法 通过建立HPLC指纹图谱和有效成分含量测定方法,对来自10个产地的枳壳药材进行分析。色谱条件为Alltima C₁₈色谱柱(4.6 mm×250 mm, 5 μm;流动相为乙腈-0.1％十二烷基磺酸钠和0.1％磷酸水溶液,梯度洗脱。流速为1.0 mL·min-1;指纹图谱检测波长为 224 nm,柚皮苷和新橙皮苷含量的检测波长为283 nm,辛弗林含量的检测波长为224 nm。结果 得到分离度、重现性均较好的枳壳药材HPLC指纹图谱,标示了6个共有色谱峰,对10批来自不同产地的枳壳的色谱指纹图谱进行了相似度评价;应用HPLC-DAD测定了10种枳壳样品中柚皮苷、新橙皮苷和辛弗林的含量,结果显示,不同产地枳壳药材中柚皮苷、新橙皮苷和辛弗林含量差异较大。结论 该方法简便准确,灵敏度高、重复性好,可以作为枳壳药材的质量控制方法。不同产地的枳壳药材有效成分(柚皮苷、新橙皮苷和辛弗林含量具有明显差异。     

Safety,Efficacy, and Mechanistic Studies Regarding Citrus aurantium (Bitter Orange) Extract and p‐Synephrine

Citrus aurantium L. (bitter orange) extracts that contain p‐synephrine as the primary protoalkaloid are widely used for weight loss/weight management, sports performance, appetite control, energy, and mental focus and cognition. Questions have been raised about the safety of p‐synephrine because it has some structural similarity to ephedrine. This review focuses on current human, animal, in vitro, and mechanistic studies that address the safety, efficacy, and mechanisms of action of bitter orange extracts and p‐synephrine. Numerous studies have been conducted with respect to p‐synephrine and bitter orange extract because ephedra and ephedrine were banned from use in dietary supplements in 2004. Approximately 30 human studies indicate that p‐synephrine and bitter orange extracts do not result in cardiovascular effects and do not act as stimulants at commonly used doses. Mechanistic studies suggest that p‐synephrine exerts its effects through multiple actions, which are discussed. Because p‐synephrine exhibits greater adrenergic receptor binding in rodents than humans, data from animals cannot be directly extrapolated to humans. This review, as well as several other assessments published in recent years, has concluded that bitter orange extract and p‐synephrine are safe for use in dietary supplements and foods at the commonly used doses. Copyright © 2017 The Authors Phytotherapy Research Published by John Wiley & Sons Ltd.     

基于传质数学模型研究丹参-枳实复方中成分存在状态与纳滤分离机制

目的基于传质数学模型,探索丹参-枳实复方中成分存在状态与纳滤分离机制。方法以原儿茶醛、迷迭香酸、丹酚酸B、辛弗林为指标,进行单体成分溶液及丹参-枳实复方溶液纳滤分离,收集膜通量与指标成分截留率,基于传质模型中传质系数与溶质浓度的幂值相关性,以单一成分为参照,拟合复方溶液中成分存在状态,探讨纳滤分离机制。结果分离压力与膜通量呈正性相关,指标成分在单体溶液和复方溶液中传质系数与浓度幂值相关性高,回归系数均大于0.98,纳滤传质模型成立。通过单一成分传质特征构建复方溶液中成分状态解析模式,丹参-枳实复方溶液中指标成分以复合态存在的比例为原儿茶醛26.17%、迷迭香酸79.87%、丹酚酸B89.15%,辛弗林96.92%。结论构建了复方溶液的成分存在状态解析模式,阐明了丹参-枳实复方提取液纳滤分离机制,为中药成分分离精制提供技术支撑。     

Safety evaluation of p‐synephrine following 15 days of oral administration to healthy subjects: A clinical study

Extracts of bitter orange (BOE, Citrus aurantium L.) and its primary protoalkaloid p‐synephrine are extensively consumed as dietary supplements. p‐Synephrine is also present in foods and juices prepared from various Citrus species. The safety of p‐synephrine has been questioned as a result of structural similarities with ephedrine. This study assessed the cardiovascular (stimulant) and hemodynamic effects of BOE (49 mg p‐synephrine) daily given to 16 healthy subjects for 15 days in a placebo‐controlled, cross‐over, double‐blinded study. A physical evaluation by a cardiologist, as well as heart rates, blood pressures, and electrocardiograms were determined, and blood samples were drawn at baseline, and Days 5, 10, and 15. Serum levels for caffeine and p‐synephrine were measured at 1 and 2 weeks. Subjects completed a 10‐item health and metabolic questionnaire at baseline and on Day 15. No significant changes occurred in heart rate, electrocardiograms, systolic blood or diastolic pressures, blood cell counts, or blood chemistries in either the control or p‐synephrine treated groups at any time point. No adverse effects were reported in response to the bitter orange (p‐synephrine). Caffeine consumed by the participants varied markedly. Under these experimental conditions, BOE and p‐synephrine were without stimulant (cardiovascular) and adverse effects.     

Cardiovascular Safety of Oral p‐Synephrine (Bitter Orange) in Healthy Subjects: A Randomized Placebo‐Controlled Cross‐over Clinical Trial

Bitter orange (Citrus aurantium) extract and its primary protoalkaloid p‐synephrine are widely consumed in combination with multiple herbal ingredients for weight management and sports performance. p‐Synephrine is also present in juices and foods derived from a variety of Citrus species. Questions exist regarding the safety of p‐synephrine because of structural similarities with other biogenic amines. This study assessed the cardiovascular (stimulatory) effects of bitter orange extract (49‐mg p‐synephrine) given to 18 healthy subjects (nine men and nine women) in a double‐blinded, placebo‐controlled cross‐over study. Heart rates, blood pressures, and electrocardiograms were determined at baseline, 30, 60, 90 min, 2, 4 , 6, and 8 h. Blood samples were drawn at baseline, 2 h and 8 h for serum chemistries, blood cell counts, and p‐synephrine and caffeine levels. No significant changes occurred in electrocardiograms, heart rates, systolic blood pressure, blood chemistries, or blood cell counts at any time point in either control or p‐synephrine treated group. A small (4.5 mmHg) decrease in diastolic blood pressure occurred in the p‐synephrine treated group at 60 min. No adverse effects were reported. Caffeine ingestion varied markedly among the participants. p‐Synephrine does not act as a stimulant at the dose used. Copyright © 2016 John Wiley & Sons, Ltd.