壮腰健肾丸宏量及微量元素的测定及其意义

用等离子体原子发射光谱法测定了壮腰健肾丸中１８种宏量及微量元素的含量，并对微量元素与壮腰健肾丸疗效之间的关系作了探讨。     

Simultaneous determination of eight bioactive components of Qishen Yiqi dripping pills in rat plasma using UFLC–MS/MS and its application to a pharmacokinetic study

In this study, a rapid and reliable ultra‐fast liquid chromatography–tandem mass spectrometry method was developed and validated for the simultaneous determination of eight active ingredients, including astragaloside IV, ononin, tanshinol, protocatechualdehyde, protocatechuic acid, salvianolic acid D, rosmarinic acid and ginsenoside Rg₁, in rat plasma. The plasma samples were pretreated by protein precipitation with acetonitrile. Chromatographic separation was performed on a Waters Acquity UPLC® BEH C₁₈ column (1.7 μm particles, 2.1 × 100 mm). The mobile phase consisted of 0.1% aqueous formic acid (A)–acetonitrile with 0.1% formic acid (B) at a flow rate of 0.4 mL/min. Quantification was performed on a triple quadruple tandem mass spectrometry with electrospray ionization by multiple reaction monitoring both in the negative and in the positive ion mode. The lower limit of quantification of tanshinol was 2.0 ng/mL and the others were 5.0 ng/mL. The extraction recoveries, matrix effects, intra‐ and inter‐day precision and accuracy of eight tested components were all within acceptable limits. The validated method was successfully applied to the pharmacokinetic study of the eight active constituents after intragastric administration of three doses (1.0, 3.0, 6.0 g/kg body weight) of Qishen Yiqi Dripping Pills to rats.     

用缩醛树脂制作光学抛光片

本文讨论了缩醛树脂一般性质和特性，及其在制作光学抛光片中的应用。     

刺五加叶黄酮脂质体和滴丸的药动学差异比较

采用液质联用(LC-MS/MS)方法,分析刺五加叶黄酮脂质体、刺五加叶滴丸和刺五加叶黄酮提取物经大鼠灌胃给药后其主要成分金丝桃苷的药代动力学和生物利用度,考察刺五加叶黄酮的适宜剂型。用PKsolver软件进行药代动力学数据处理,大鼠灌胃刺五加叶黄酮提取物、刺五加叶滴丸和刺五加叶黄酮脂质体后测得金丝桃苷的最大血药浓度(C_(max))分别为(210.24±10.3)、(254.12±9.2)、(349.34±12.5)μg/L;0~t时间内药时曲线面积(AUC_(0-t))分别为(30.7±2.7)、(35.01±1.98)、(45.2±2.8)μg/(m L·min);平均驻留时间(MRT)分别为(334.42±75.36)、(394.56±90.26)和(640.35±84.26)min。结果表明,刺五加叶黄酮脂质体血药达峰浓度增加,清除速率降低,药时曲线下面积加大,生物利用度显著提高,脂质体有望成为刺五加叶黄酮的适宜剂型。     

The Double Face of Ketamine—The Possibility of Its Identification in Blood and Beverages

The purpose of this study was to develop and validate a high-sensitivity methodology for identifying one of the most used drugs—ketamine. Ketamine is used medicinally to treat depression, alcoholism, and heroin addiction. Moreover, ketamine is the main ingredient used in so-called “date-rape” pills (DRP). This study presents a novel methodology for the simultaneous determination of ketamine based on the Dried Blood Spot (DBS) method, in combination with capillary electrophoresis coupled with a mass spectrometer (CE-TOF-MS). Then, 6-mm circles were punched out from DBS collected on Whatman DMPK-C paper and extracted using microwave-assisted extraction (MAE). The assay was linear in the range of 25–300 ng/mL. Values of limits of detection (LOD = 6.0 ng/mL) and quantification (LOQ = 19.8 ng/mL) were determined based on the signal to noise ratio. Intra-day precision at each determined concentration level was in the range of 6.1–11.1%, and inter-day between 7.9–13.1%. The obtained precision was under 15.0% (for medium and high concentrations) and lower than 20.0% (for low concentrations), which are in accordance with acceptance criteria. Therefore, the DBS/MAE/CE-TOF-MS method was successfully checked for analysis of ketamine in matrices other than blood, i.e., rose wine and orange juice. Moreover, it is possible to identify ketamine in the presence of flunitrazepam, which is the other most popular ingredient used in DRP. Based on this information, the selectivity of the proposed methodology for identifying ketamine in the presence of other components of rape pills was checked.     

冠心苏合丸中挥发性组分的分析及主成分冰片的测定

采用同时蒸馏-萃取法提取冠心苏合丸中的挥发性组分,测得两种冠心苏合丸中的挥发性组分含量分别为14％和9．8％。利用GC-MS方法对两种冠心苏合丸所得的挥发性组分进行分析,通过检索NIST98谱图库,并结合标准谱图库和有关文献,从冠心苏合丸的挥发性组分中分别确定出14、19种化学成分,分别占挥发性组分总检出量的97．24％和98．76％。用峰面积归一化法,得出各化学成分在挥发性组分中的相对百分含量。主要挥发性组分是冰片。并采用气相色谱法对冠心苏合丸中冰片的含量进行了测定冰片质量浓度在1．0～5、0mg／mL范围内成良好的线性关系,冰片的平均回收率为98％～106％。     

怀菊花中微量铁的测定

为探讨邻二氮菲分光光度法测定怀菊花中微量元素铁含量的可行性,怀菊花的药理功效、食用营养价值与微量元素含量可能存在的关系,根据铁离子与特定显色剂显色产生可见吸收,采用混合酸y（HNO3）：V（HClO4）=4＋1对怀菊花样品湿法消化处理,在pH2～9的溶液中试剂与铁生成稳定的橙色络合物,并用分光光度法测定了怀菊花中微量元素铁含量。结果表明,所选的怀菊花中铁含量303．9～337．9μg／g,加标回收率为90．2％～100．6％。分光光度法操作简便、干扰离子少,测量快速、结果准确度和灵敏度高,易推广和 普及使用。     

六味地黄丸三维同步荧光光谱特性的研究

应用英国Edinburgh公司FLS920P荧光光谱仪,实验测定了六味地黄丸组分中熟地黄、山茱萸、山药、泽泻、茯苓、牡丹皮等六味中药的三维同步荧光光谱,并提取荧光特征参数,发现六味中药均为荧光物质,谱图线形各不相同,具有指纹特性,且与药理相吻合。进一步,实验测定六味地黄丸的标准水煎剂及非标准水煎剂的三维同步荧光光谱,发现两者差异明显,可用于区分不同组方的中成药水煎剂。实验与理论均表明：将三维荧光光谱分析方法与同步荧光光谱分析方法相结合,可以进一步提高荧光光谱技术的灵敏度和选择性,在多组分复杂混合物的荧光光谱分析中有明显的优势。因此,本文的工作为建立完整信息中药材指纹图谱提供了一种方便快捷可靠的方法,也可为中成药的品质鉴别和成分分析提供帮助。     

浓缩当归丸的提取工艺研究

采用索氏提取法提取浓缩当归丸的有效成分阿魏酸，同时用正交分析法对提取溶剂种类、用量及提取时间进行考察，最后以高效液相色谱法(HPLC)测定阿魏酸的含量，从而筛选出最佳提取工艺．结果显示：选用60mLV甲醇：V甲酸=95：5的混合液作为提取溶剂．预先浸泡24h，再索氏提取3h，得到浓缩当归丸的有效成分阿魏酸的含量最高．     

高效毛细管电泳同时分离测定栀子苷、芍药苷及丹皮酚的研究

建立了同时分离测定栀子苷、芍药苷和丹皮酚的高效毛细管电泳新方法.以十六烷基三甲基溴化铵为表面活性剂形成胶束、甲醇作为有机改性剂、 NaOH溶液为背景电解质,在234 nm 波长下紫外检测.对十六烷基三甲基溴化铵、 NaOH的浓度以及有机改性剂、分离电压等因素对分离的影响做了系统的研究, 确立了栀子苷、芍药苷和丹皮酚的最佳分离条件.栀子苷、芍药苷、丹皮酚分别在20～100 μg/mL,5～80 μg/mL,2～20 μg/mL范围内呈较好的线性关系,回收率分别为99.00%～100.27%,99.49%～101.83%,97.11%～99.06%.方法已用于加味逍遥丸中3种成分的检测.