HPLC测定不同产地麻黄中盐酸麻黄碱的含量

目的:测定不同产地麻黄中盐酸麻黄碱的含量.方法:采用高效液相色谱法,C18固定相,流动相为乙腈-0.02mol/L磷酸二氢钾(含0.2%三乙胺,用磷酸调PH为2.5)(3:97),流速为1.2ml/min,检测波长为210nm.结果:产于内蒙通辽的麻黄盐酸麻黄碱含量最高,达1.1202%;产于新疆乌鲁木齐的麻黄含量最低,为0.3293%.结论:不同产地的麻黄盐酸麻黄碱的含量有较大差异.所建立的HPLC方法快捷、灵敏、适用性良好.     

HPLC法测定不同产地麻黄中麻黄碱的含量

目的：建立高效液相色谱法测定不同产地麻黄中麻黄碱的含量方法。方法：高效液相色谱法,色谱柱为IN-ERTSIL ODS-SP柱（4.6 mm×150 mm,5μm）;流动相：乙腈-（0.02 mol/L磷酸二氢钾＋0.02%三乙胺＋0.2%磷酸水溶液）（10∶90）;流速：1 ml/min;检测波长：205 nm。结果：线性范围为0.2～0.8μg（r=0.999 7）,回收率为98.21%,RSD为0.79%;不同产地麻黄中麻黄碱含量差异较大,以山西麻黄含量最高。结论：以HPLC法测定麻黄中麻黄碱的含量,精密度高,操作简便,为选择麻黄道地药材提供可靠依据。     

麻黄常规粉体与超微粉体中麻黄碱在小鼠肺部药物浓度的比较研究

目的测定麻黄常规粉体与超微粉体中麻黄碱在小鼠肺部的浓度,探讨不同粒径麻黄粉体对麻黄碱在小鼠肺部浓度的影响。方法小鼠以相同剂量灌胃给予常规与超微2种麻黄粉体后,在规定的时间点摘取肺,匀浆处理后用HPLC法测定其中麻黄碱的含量。结果超微粉体组肺内麻黄碱含量明显高于常规粉体组。结论超微粉体可提高麻黄药物在小鼠肺内的药物浓度。     

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。     

玉黄感冒冲剂有效成分麻黄碱的含量测定

目的:建立玉黄感冒冲剂中主药麻黄的有效成分麻黄碱的含量测定方法。方法:用酸性染料染色—分光光度法测定玉黄 感冒冲剂中麻黄碱的含量。结果:盐酸麻黄碱加样回收率为97.91%,RSD为2.15%(n=5)。结论:该法操作准确,重现性好,可作 为该产品中麻黄碱的含量测定方法。     

麻黄及其制剂中麻黄碱的含量测定

目的：探讨用气相色谱法测定麻黄及其制剂中麻黄碱的含量。方法：以ＯＶ－１７为固定液,柱温160℃,联吡啶为内标物,以ＦＩＤ检测器 黄及其含麻黄的９种成药制剂中麻黄碱的含量。结果：麻黄三在０.２５－３.５μg范围内呈良好的线性关系。对麻黄和小儿治咳糖浆的加样加收率分别为１００.１％和１０３.０％,ＲＳＤ分别为１.５％和２.２％。结论：本法简便、快速、准确,可作为麻黄及一些制剂的质量控制方法。     

HPLC法测定小儿清热止咳泡腾片及麻黄中盐酸麻黄碱的含量

目的:建立测定小儿清热止咳泡腾片中盐酸麻黄碱含量的方法.方法:采用HPLC法,以优选的乙腈-水-磷酸-三乙胺(3: 97 : 0.1 : 0.1)为流动相;检测波长为205nm,测定了小儿清热止咳泡腾片麻黄中盐酸麻黄碱的含量.结果:盐酸麻黄碱色谱峰峰形对称,且与杂质峰获得了完全分离,精密度、重现性及回收率实验等均符合要求,并用此方法考察了药材麻黄中盐酸麻黄碱含量.结论:方法准确性好、操作简便,可用于盐酸麻黄碱的含量控制.     

咳喘宁颗粒中麻黄碱的含量测定

咳喘宁颗粒为中药复方制剂 ,由麻黄、杏仁、栝楼等 12味中药组成。具有宣肺、止咳、平喘、祛痰之功效。麻黄为方中主药 ,其主要成分为麻黄碱。本文用酸性染料比色法对麻黄碱的含量进行了测定 ,为控制本品内在质量提供实验依据。1 仪器与材料ＵＶ - 2 6 0型紫外可见分光光度计 (     

HPLC法测定克咳胶囊中盐酸麻黄碱的含量

克咳胶囊收载于部颁标准[1],由麻黄、罂粟壳、甘草等七味药组成复方制剂。麻黄为本品君药,其所含成分麻黄碱为该制剂中主要有效成分之一,部颁标准中没有对其进行含量控制的方法。目前测定盐酸麻黄碱含量的方法有酸碱滴定法[2]、高效液相色谱法[3],但用于本品的含量测定时效果却不好。为了提高克咳胶囊的质量标准,本文通过研究比较,建立了高效液相色谱法测定克咳胶囊中盐酸麻黄碱的含量,取得了满意的效果,为制定克咳胶囊中有效成分的含量测定方法,提供了新的依据。1仪器与试药HP-1100高效液相色谱仪,二极管阵列检测器,HP化学工作站。盐酸麻…     

高效液相色谱法测定止咳祛痰颗粒中盐酸麻黄碱的含量

止咳祛痰颗粒为中药桔梗、百部、苦杏仁等与盐酸麻黄碱制成的复方制剂,盐酸麻黄碱是中药麻黄的主要有效成分。现代药理研究表明,盐酸麻黄碱具有广泛的生理活性如拟肾上腺素能神经作用,对呼吸系统具有平喘、镇咳、发汗、利尿、抗变态、抗炎、解热、抗病原微生物作用等,其中对呼吸系统的作用、抗变态作用与止咳祛痰颗粒功能主治密切相关。原制剂标准尚未有含量测定,故我们用高效液相法建立了盐酸麻黄碱的含量测定,从而有效地对止咳祛痰颗粒进行质量控制,获得满意效果。     

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。     

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。     

Studies on cultivated ephedra plants in inner mongolia autonomous region and ningxia hui autonomous region

Progression of the desertification in northern China has been causing damage to wild Ephedra plants on which we depend for most of supply of the traditional herbal medicine, "Ma huang." The Chinese government encourages the cultivation of Ephedra plants, and Ephedra fields have been reclaimed in the original Ephedra habitats in recent years. We surveyed 7 Ephedra fields that have been recently developed in the Inner Mongolia Autonomous Region and Ningxia Hui Autonomous Region to collect information on Ephedra plant cultivation, especially pertaining to crop species. Specimens taken from those Ephedra fields were genetically and morphologically analyzed, and their ephedrine alkaloid content was examined. DNA analyses of Ephedra specimens, including DNA sequencing of ITS (internal transcribing sequence of nuclear ribosomal DNA) and trn L/F (intron of trnL and intergenic spacer between the trnL and trnF of chloroplast DNA) region and species-specific amplification of trn L/F were conducted to identify Ephedra species. Based on the results of DNA sequencing and morphological determination, the crops grown in 6 fields ware identified as Ephedra sinica, while co-planting of E. sinica and E. intermedia was found in one field where a higher appearance rate of plants with varied morphology from wild Ephedra plants was observed. Furthermore, direct sequencing of the PCR product of the trn L/F region of some specimens from the field and their species-specific PCR showed ambivalent result. Cloning and sequencing of the PCR product of the trn L/F region of those specimens DNA suggested their heteroplasmy, containing both E. sinica- and E. intermedia-type chloroplasts. On the other hand, the profile of the ephedrine alkaloid content was clearly correlated with the result of direct sequencing of the trn L/F region; the specimens showing the E. sinica-type sequence contained more ephedrine than pseudoephedrine, and the specimens of the E. intermedia-type more pseudoephedrine.     

Survey on resources of Ephedra plants in Xinjiang

The resources of wild Ephedra plants in the Xinjiang Uygur Autonomous Region were surveyed. Ephedra plants mainly grow on the fringes of the Taklimakan Desert and Gureban-tonggute Desert. We found six genotypes of Ephedra przewalskii growing widely in Xinjiang. Three genotypes of Ephedra intermedia were limited to the northern and eastern parts, and Ephedra regeliana scattered in the northern part of Xinjiang. These Ephedra specimens were analyzed for DNA sequences of nuclear ribosomal DNA, internal transcribed spacers 1 and 2, chloroplastic DNA, trnL intron and trnL-trnF intergenic spacer. Intraspecific variation of the nucleotide sequence in E. przewalskii was found in different habitats. Norephedrine, ephedrine, pseudoephedrine, and methylephedrine contents of the specimens were determined. Although Ephedra intermedia of all three genotypes contained ephedrine alkaloids, ephedrine alkaloids were not detected in E. regeliana and E. przewalskii.     

Genetic diversity of Ephedra plants in mongolia inferred from internal transcribed spacer sequence of nuclear ribosomal DNA

Ephedrae herba has been used for treating colds, relieving coughs and asthma from ancient times. We previously reported the distribution of Ephedra sinica, E. equisetina, E. przewalskii, E. regeliana, E. monosperma and Ephedra sp. in Mongolia, and among them E. sinica and E. equisetina were potential new resources of Ephedrae herba of Japanese pharmacopoeia grade, based on our field survey and subsequent molecular and chemical assessments. However, the Ephedra population in southwestern areas showed a high possibility of having hybrid origins. Further field surveys in southwestern areas, and sequence analysis of the partial nuclear internal transcribed spacer 1 (ITS1) region, besides trnK and 18S ribosomal RNA (rRNA) gene regions, were conducted in order to obtain detailed evidence of hybridization status. As a result, the distribution of E. glauca in western area and E. lomatolepis in western-most area was confirmed. The ITS sequences from all 8 Ephedra species collected in Mongolia were roughly divided into 5 types (types I-V). Type II sequence, having several additive nucleotides, was found in Ephedra sp., E. glauca, E. regeliana and E. sinica, which provided useful information for tracing hybrid origins. Morphological, genetic and distribution evidence suggested that the hybridization of Ephedra species occurred widely in southwestern Mongolia, and several Ephedra species including E. przewalkskii and E. intermedia were involved in these events. Integrated with our previous report, trnK-, 18S- and ITS-types from pure lines of each species are proposed. In addition, we propose a practicable method for detecting additive peaks on a direct sequencing electropherogram.     

鼻炎通窍喷雾剂的质量标准研究

目的:建立鼻炎通窍喷雾剂的质量标准。方法:采用薄层色谱法对麻黄、黄芩、白芷进行定性鉴别;用高效液相色谱法测定盐酸麻黄碱和黄芩苷的含量。结果:麻黄、黄芩、白芷的薄层色谱图斑点清晰,阴性无干扰。盐酸麻黄碱进样量在0.0798μg~1.1172μg浓度范围内与峰面积线性关系良好,平均回收率为97.26%,RSD为2.33%(n=6);黄芩苷进样量在0.1364μg~2.046μg浓度范围内与峰面积线性关系良好,平均回收率为98.15%,RSD值为2.03%(n=6)。结论:所用方法专属性强,灵敏度高,重现性好,可用于鼻炎通窍喷雾剂的质量控制。     

Determination of ephedrine alkaloids in Ephedra natural products using HPLC on a pentafluorophenylpropyl stationary phase

In this study a pentafluorophenylpropyl (PFPP) stationary phase was applied to the fast and reliable qualitative and quantitative analysis of ephedrine alkaloids in Ephedra plant material and derivatives. A Discovery HS F5 column (150mmx4.6mm i.d., 5microm) was used, with an isocratic mobile phase composed of ammonium acetate (7mM) in acetonitrile-water (90:10, v/v), at a flow rate of 1.0ml/min. The column temperature was set at 45 degrees C. UV detection was set at 215 and 225nm. The total analysis time was 16min. The validation parameters, such as linearity, sensitivity, accuracy, precision and specificity, were found to be highly satisfactory. Sonication and microwave extractions were compared in order to optimize the yield of the target analytes. Under the optimized extraction conditions (based on two cycles of sonication with methanol at 40 degrees C for 15min), different matrices containing Ephedra were successfully analyzed for their alkaloid content. The method was applied to the analysis of standard reference materials (SRMs) containing Ephedra. Furthermore, the developed technique allowed the simultaneous determination of ephedrine alkaloids and synephrine, the main phenethylamine alkaloid of Citrus aurantium, that has replaced Ephedra in dietary supplements used in the treatment of obesity. The results indicated that this procedure is suitable for the phytochemical analysis of Ephedra plant material and extracts, and can be applied to demonstrate the label claims for product content, including the absence of ephedrine alkaloids in Ephedra-free products.     

麻黄软胶囊的溶出稳定性及影响因素考察

目的：考察中药麻黄软胶囊的溶出稳定性及影响因素,探讨中药软胶囊溶出迟缓机制。方法：采用加速试验,评价麻黄软胶囊的溶出稳定性;以平衡溶胀量和ε-氨基酸残基含量为指标,评价明胶囊壳的交联程度;应用红外光谱和醛类专属反应,鉴定麻黄提取物中醛类成分,并测定其含量。结果：在加速试验条件下（40℃,75％相对湿度）,放置30天后,明胶囊壳的平衡溶胀量和ε-氨基酸残基含量均显著下降（P〈0．01）,其交联度显著增加（P〈0．01）;放置60天后,麻黄软胶囊溶出度显著下降（P〈0．01）。环境因素（高温／高湿）、溶媒介质（聚乙二醇）和药物成分（麻黄提取物）均可导致明胶交联度显著提高（P〈0．01）,其中麻黄提取物的作用明显大于另两种影响因素。麻黄提取物中醛质量分数达约1．6％。结论：麻黄软胶囊溶出迟缓与囊壳明胶发生交联反应有关,而麻黄提取物中醛类成分是促进软胶囊发生交联反应、导致其溶出迟缓的主要原因。     

Ephedra alkaloid contents of Chinese herbal formulae sold in Taiwan

Consumption of Ephedra alkaloids is prohibited in‐competition by the World Anti‐Doping Agency (WADA). In Taiwan, colds are often treated with Chinese herbal formulae containing Herba Ephedrae. We screened products sold in Taiwan and preliminarily assessed their relationships with WADA threshold violations. Fifty‐six concentrated powder products, including 19 Chinese herbal formulae that contained Herba Ephedrae, were collected. The content of Ephedra alkaloids, namely ephedrine (E), methylephedrine (ME), norpseudoephedrine (NPE; cathine), pseudoephedrine (PE), and norephedrine (NE; phenylpropanolamine), was determined using a validated high‐performance liquid chromatography method. The results revealed that the phenotypic indicators of the collected products, E/PE and E/total ratios, were 1.52–4.70 and 0.49–0.72, respectively, indicating that the Herba Ephedrae species in these products was probably E. sinica or E. equisetina, but not E. intermedia. The contents of E, ME, NPE, PE, and NE and the total alkaloid contents in the daily doses of the products were 0.45–34.97, 0.05–4.87, 0.04–3.61, 0.15–12.09, and 0.01–2.00 mg and 0.68–53.64 mg, respectively. The alkaloid contents followed a relatively consistent order (E > PE > ME ≈ NPE > NE), even for products from different manufacturers. We calculated that single doses of 50.0% and 3.6% of the products would result in the WADA thresholds of E and NPE being exceeded, respectively. Our data provide critical information for athletes and medical personnel, who should be wary of using complex Chinese herbal formulae in addition to over‐the‐counter products.     

The use of polymerase chain reaction (PCR) for the identification of ephedra DNA in dietary supplements

As part of a continuing research effort to develop chemical and genetic authentication profiles of botanicals, an investigation was performed with the goal to detect, identify and verify Ephedra sinica Stapf DNA in dietary supplements such as plant mixtures and tablets/capsules. We amplified and sequenced the chloroplast psbA-trnH spacer from 21 Ephedra spp. and from two of their closest relatives, Gnetum gnemon L. and Welwitschia mirabilis Hook. Based on sequence comparisons, we identified regions unique to all of the Ephedra spp. samples analyzed. We concluded that the psbA-trnH spacer sequence could be used as a molecular marker. Based on this spacer sequence, we designed Ephedra spp.-specific primers that can help to identify Ephedra spp. DNA in plant mixtures containing as little as 1/1,000 part of Ephedra spp. tissue. We used a DNA extraction method that allows for quick DNA isolation from plant mixtures for PCR analysis.