炮山甲内掺假的鉴别

目的 防止掺假炮山甲进入临床使用.方法 在入库前验收时,把完整的和打碎的炮山甲分别用鼻闻、手摸、眼看、口尝等传统方法进行鉴别,发现有可疑的再用理化方法进行氯化物、钠盐、硫酸盐、铝盐、钾盐、苯甲酸、谷氨酸的鉴别反应怍进一步鉴别,以确定掺假物性质.结果 目前发现不法商贩把食盐、硫酸盐、铝盐、苯甲酸钠、味精掺入炮山甲内,以增加重量.结论 掺假炮山甲单凭传统性状鉴别较难判定,需结合理化方法识别炮山甲是否掺假和掺假物类别.     

盐矾掺伪的炮山甲鉴别

目的:正确鉴别盐矾掺伪的炮山甲.方法:采用性状鉴别及理化鉴别.结果与结论:鉴别盐矾掺伪炮山甲的方法简便易行,可确保炮山甲的质量,使患者用药安全有效.     

炮山甲的HPLC指纹图谱研究

目的:建立炮山甲的高效液相色谱(HPLC)指纹图谱。方法:采用HPLC法。色谱柱为Capcell Pak MgⅡS5 C18,流动相为乙腈-0.1%磷酸溶液(梯度洗脱),流速为0.8 m L/min,检测波长为275 nm,柱温为30℃,进样量为10μL。以酪氨酸为参照,测定11批药材的HPLC图谱,采用《中药色谱指纹图谱相似度评价系统》(2004 A版)进行共有峰指认和相似度评价。结果:11批炮山甲药材的HPLC图谱有23个共有峰,相似度均>0.90。经验证,11批药材样品HPLC图谱与对照指纹图谱具有较好的一致性。结论:该研究所建HPLC指纹图谱可为炮山甲的鉴别和质量评价提供参考。     

牛黄及其伪品的鉴别

因天然牛黄紧缺,价格昂贵,常有掺假牛黄。本文采用性状鉴别,显微鉴别,理化鉴别方法。鉴别牛黄的真品及常见伪品。方法简便易行,有助于保证牛黄临床应用的安全。     

乳香的商品调查与质量检测方法研究

目的对市售乳香及其炮制品进行调查鉴定,并研究其掺伪品中所含松香酸的检测方法。方法从国内10个省市的药材市场中收集样品50批,采用性状、理化、TLC、HPLC-PAD、HPLC-MS等方法对其中的掺伪成分淀粉、松香酸进行定性定量分析。结果经检测50批市售品,其中只有27批为正品;23批掺伪品中有13批检出淀粉,22批检出松香酸。结论市售乳香质量问题较严重,主要是用淀粉、松香掺假,或在正品中掺入伪品,本实验所建立的检测方法,可用于掺伪物松香定性定量检测。     

炮山甲与劣品炮大甲片的经验鉴别

目的：辨清炮山甲真伪,杜绝劣质炮大甲片。方法：对正品炮山甲与劣品炮大甲片在性状、颜色、大小等方面进行比较。结果：正品炮甲片长宽各0.75~5.50 cm,金黄色或黃褐色,质酥脆,易折断,断面厚0.2~0.4 cm;而劣品炮大甲片长宽各6~10 cm,是正品的3~5倍,黄褐色至棕黄色,质酥不脆,能折断,断面厚0.6~1 cm。结论：性状特征能区别开炮大甲片。     

药用植物鸢尾的生药学研究

目的:对鸢尾根茎进行系统的生药学研究,为其进一步开发利用提供鉴别依据。方法:用传统方法对药材性状进行鉴别;用徒手切片法对其根茎进行切片并观察;粉末显微特征观察;用薄层色谱和紫外光谱进行理化鉴别。结果:详细描述了鸢尾根茎的生药性状、横切面构造、粉末特征以及分析了理化鉴别的研究结果。结论:试验结果可为鸢尾根茎的生药鉴定、质量标准制定及进一步开发利用提供参考依据。     

几种常见中药饮片掺伪、掺杂鉴别及快速检验

目的掌握几种易掺伪中药饮片的掺假情况以及对掺假的识别方法和快速检验方法。方法以来源、性状与正品的典型特征进行比较,同时结合薄层色谱和杂质等检验项目进行判断。结果与结论用简单的方法可快速鉴别出药材真伪,同时结合相应的检验项目,可判定中药饮片合格与否,从而杜绝掺伪掺杂饮片进入临床。     

微波加热炮制王不留行和芥子的可行性研究

目的 探讨用微波加热炮制王不留行、芥子的可行性。方法 用微波炮制法和药典清炒法制备2种炮制品,比较2种炮制品的外观性状;用薄层色谱（TLC）法对微波炮制品和清炒品进行定性鉴别;用药典方法对两药的不同炮制方法进行浸出物测定;用高效液相色谱（HPLC）法分别对其中的王不留行黄酮苷、芥子碱硫氰酸盐进行含量测定。结果 2种炮制品的外观均能达到药典对该品种的要求;TLC表明2种炮制品中都能出现与对照品和对照药材相同颜色的斑点;浸出物测定表明,微波法比清炒法炮制品的浸出物含量高;HPLC表明,2个品种微波炮制品的王不留行黄酮苷及芥子碱硫氰酸盐含量测定均高于传统清炒法。结论 微波炮制法优于传统清炒法,值得深入研究和大力推广。     

穿山甲及炮制品的真伪鉴别

目的鉴别穿山甲及炮制品的真伪。方法查阅相关文献,结合实践工作经验,通过外观性状、理化鉴定、显微鉴定,进行对比。结果正品与伪品存在明显差异。结论伪品不能作正品入药,必须重视真伪鉴别,确保临床用药安全有效。     

LC-DAD-MS／MS法检测抗风湿中药制剂中非法添加的双氯芬酸盐

目的：采用液相色谱-二极管阵列-串联质谱检测法（LC—DAD—MS／MS）定性、定量检测某抗风湿中药中非法添加的双氯芬酸盐。方法：选用Agilent ZORBAX SB C18（150mm×4．6mm,5μm）柱,以甲醇-20mmol·L^-1乙酸铵溶液（60：40）为流动相,对非法制剂的提取液进行分析。通过与对照品的色谱保留时间、紫外吸收光谱及质谱碎裂行为的比较,对此类药进行定性鉴别和定量测定。结果：某抗风湿中药胶囊荆两个批次均检测到了西药双氯芬酸盐。结论：所用方法专属性强、灵敏度高、操作简便,可作为分析中药中非法添加双氯芬酸盐的参考方法。     

对《中国药典》2010年版利巴韦林注射液有关物质检查方法的探讨

目的：对利巴韦林注射液有关物质检查方法进行探讨。方法：按照《中国药典》2010年版二部利巴韦林注射液有关物质检查的方法,对利巴韦林注射液进行破坏性试验,同时对利巴韦林的降解产物进行考察。结果：利巴韦林杂质峰与氯化钠峰难以分开。因此,利巴韦林注射液处方中如有氯化钠的存在,将干扰利巴韦林注射液有关物质的检查。结论：建议有关物质检测时扣除氯化钠峰的影响,或者企业在利巴韦林注射液的处方中标注氯化钠的量或不加氯化钠。     

替卡西林钠的合成新工艺

目的:制备替卡西林钠。方法:以3-噻吩丙二酸为起始原料,经过酰氯化、酰胺化、成盐反应制得替卡西林单钠。替卡西林单钠与碳酸氢钠在水溶液中反应后,真空冷冻干燥制得替卡西林钠。结果:总收率62.8%,含量>98.0%。结论:该方法制备的替卡西林钠收率高,质量好,易于实现工业化。     

HPLC法测定左旋泮托拉唑钠肠溶微丸的含量和有关物质

目的测定左旋泮托拉唑钠肠溶微丸胶囊的含量和有关物质。方法建立HPLC法,色谱柱:DiamonsilTMC18(5μm,4.6 mm×250 mm),流动相:乙腈-磷酸盐缓冲液(取磷酸氢二钠1.12 g,磷酸二氢钠0.18 g,加水溶解并稀释至1 000 mL,调pH值至7.6)(体积比为30∶70),检测波长:288 nm。结果左旋泮托拉唑在20.0~100.0 mg.L-1内线性关系良好,r=0.999 6,平均回收率为99.3%(n=9),RSD%=0.54。结论方法可用于制剂的含量和有关物质测定。     

Control of salt intake by steroids and cerebral peptides.

Steroids (aldosterone and testosterone) and peptides of cerebral origin (angiotensin II and the tachykinins) control the salt intake of the rat. They arouse or suppress the behaviour and produce life-long enhancements of NaCl intake. Need-induced salt intake (salt appetite or salt hunger), which is the consequence of sodium deficiency, is aroused by a synergy within the brain of cerebral angiotensin II and aldosterone. And prior episodes of sodium depletion produce enhancements of subsequent salt appetites, but only if the prior depletions were accompanied by angiotensin II and aldosterone action. Need-free salt intake, which occurs daily when the rat is in positive sodium balance, is inherently high in the rat and is organized in the perinatal period by aromatized testosterone which suppresses the intake of the male. It is also enhanced by prior activations of angiotensin II and aldosterone. Both need-induced and need-free salt intake are suppressed by intracranial tachykinins. Non-mammalian tachykinins (eledoisin, physalaemin, kassinin) are both antidipsogenic and antinatriorexigenic, but amino-senktide, an analogue of the mammalian tachykinin substance P with selective affinity for the NK 3 receptor, appears to be a selective antinatriorexigenic agent, and could provide a rational therapy for chronic overconsumption of salt.     

A HILIC method for the analysis of tromethamine as the counter ion in an investigational pharmaceutical salt

A hydrophilic interaction chromatography (HILIC) method using an aminopropyl stationary phase was developed and validated to determine the content of tromethamine as counter ion in an investigational drug substance. Tromethamine was a very polar compound without any chromophores, and could not be readily retained and detected by conventional reserved-phase HPLC-UV methods. Furthermore, the tromethamine salt of the drug compound also had limited solubility in aqueous solution. The method employed simple acetonitrile/water mobile phase (80/20, v/v) to provide sufficient retention for tromethamine. Meanwhile, the high acetonitrile content also helped to dissolve the drug substance sample. Refractive index (RI) was used for the detection of tromethamine. The method was found to be specific without interference from the drug compound and related impurities. The method was also validated for suitable precision, linearity and accuracy for the analysis of drug substance samples. The effects of various parameters, such as acetonitrile content, mobile phase salt concentration, and column temperature on HILIC separation were investigated.     

Studies on residue on ignition test in JP

The Residue on Ignition Test specified in General Tests, Japanese Pharmacopeia is a method to measure the weight of the residual substance not volatilized when the sample is ignited under a constant condition. Generally, this test is intended to determine the content of inorganic substances contained as impurities in an organic substance, and, occasionally, to determine the amount of inorganic substances contained as components in an organic substance. Our laboratories have adopted this test method for the above two purposes in the case of the quality control for drug substances, synthetic intermediates, starting materials in the course of drug development. Some validation studies have been conducted for this test in order to clarify the quantitation limit in the case of an application for the former purpose, and trueness and precision in the case of the latter purpose. Consequently, the quantitation limit was determined as around 0.50 mg. The amount of sample should be determined based on this quantitation limit (mg) and the level of quantitation limit (%) or that of specification limit (%) should be considered from the view point of each testing purpose. The test method was also confirmed to have a good trueness and precision as the determination method for an alkaline salt, such as sodium, potassium or calcium salt, of organic compounds, as long as the test is operated with great care not to scatter the content out of crucible during ignition to incineration.     

TLC法快速筛查降糖类中成药及保健食品中添加的11种化学药品

目的建立中成药及保健食品中非法添加降糖药的定性检查方法。方法 11种化学降糖药分别采用2个薄层系统检查磺酰脲类降糖药及双胍类降糖药。结果 11种化学降糖药分离良好。结论本方法经济、快速,可用于中成药及保健食品中非法添加降糖类化学药的快速筛查。     

五合枸杞中7种微量营养素含量测定

目的:测定五合枸杞中7种微量营养素钾、钠、钙、镁、铁、锌、铜的含量.方法:采用火焰原子吸收光谱法和火焰原子发射光谱法测定待测元素的含量,选择国家小麦粉成分分析标准物质GBW(E)100195用作量值和质量监控标准,并验证测定方法的可靠性.结果:测得五合枸杞中7种微量营养素含量分别为钾29 807 mg·kg-1、钠 11 250 mg·kg-1、钙 375.25 mg·kg-1、镁 108.74 mg·kg-1、铁 98.205 mg·kg-1、锌 62.056 mg·kg-1、铜 8.227 3 mg·kg-1.结论:该测定法简便快捷、回收率好、准确度和精密度高.五合枸杞中7种微量营养素含量较高.