Enhancement of Sensitivity for Antimony Determination in Atomic Absorption Spectrophotometry by Introducing Stibine into an Argon-Hydrogen Flame

Abstract

The sensitivity of antimony determination with atomic absorption spectrophotometry is enhanced to a large extent by introducing stibine gas into an argon-hydrogen flame. As a reducing agent, zinc tablet made from the zinc powder paste with water is successfully used for quantitative and rapid productions of stibine from antimony (III) solution. The sensitivity for 1% absorption of the signal is estimated to be about 0.004 ppm of antimony.     

联立方程组新解法测定面康净片中两组分含量

采用联立方程组新解法不经提取分离直接测定面康净片中甲硝唑和维生素Ｂ６的含量。甲硝唑和维生素Ｂ６的平均回收率和相对标准偏差分别是１０１．４％，０．９７％和１００．６％，１．３１％。方法简便、快速、准确。     

CPA-矩阵法测定舒尔芬片剂中两组分的含量

本文采用ＣＰＡ－矩阵法不经分离同时测定舒尔芬片剂中双氯芬酸钠和磷酸可待因的含量。计算程序用ＢＡＳＩＣ语言编制。双氯芬酸钠和磷酸可待因的平均回收率及ＲＳＤ分别为９９．８５％，０．４６％和９９．８０％，０．５０％。方法简便、快速。     

High performance liquid chromatographic analysis of dehydroepiandrosterone and its pharmaceutical tablet formulation

A rapid, sensitive and stability indicating high performance liquid chromatographic method was developed and validated for the analysis of dehydroepiandrosterone (DHEA) in pharmaceutical tablet formulation. The analysis was done on a Supelcosil C(18) column (25 cm x 4.6 mm i.d., 5 microm). The mobile phase consisted of methanol:sodium acetate buffer solution (5 g/L):acetic acid (500 mL/L), 57:42:1, v/v/v, adjusted to pH 5 at a flow rate of 1 mL/min. Detection was carried out at a wavelength of 258 nm. The polynomial regression data for the calibration curve showed good linear relationship in the concentration range of 0.2-1 mg/mL with r = 0.9996. The method was validated for precision, accuracy and recovery. The limit of detection was found to be 50 ng/ microL. The method was applied for the analysis of DHEA in its pharmaceutical tablet formulation. The effects of different buffers and alcohols on the retention of DHEA were studied and the role of acetic acid as an organic phase modifier was also investigated.     

薄层扫描法测定利喉乐含片中没食子酸的含量

应用薄层扫描法测定了利喉乐含片中没食子酸的含量。以甲苯－醋酸乙酯－甲酸（Ｖ甲苯∶Ｖ醋酸乙酯∶Ｖ甲酸＝３∶５．４∶０．６）为展开剂,１０ｇ／ＬＦｅＣｌ３显色后,用Ｃｓ－９２０薄层扫描仪扫描,扫描波长为５２０ｎｍ。没食子酸在１．２４～６．２０μｇ之间线性关系良好,该法的加样回收率为９５．９３％,板内精密度为２．７８％,板间精密度为３．３０％,为利喉乐含片的质量控制提供了一种简便而准确的含量测定方法     

硫酸沙丁胺醇的毛细管电泳非接触电导法检测

建立了毛细管电泳-非接触电导检测分离测定硫酸沙丁胺醇的分析方法。分别考察了分离介质、背景电解质及其浓度和pH、分离电压、进样时间、激发电压、激发频率等因素对实验结果的影响。在优化的实验条件(以15 mmol/L乳酸水溶液(pH 2.7)为电泳介质,10 kV下电动进样3 s,分离电压为10 kV,激发电压为60 V,激发频率为120 kHz)下,硫酸沙丁胺醇的检出限(信噪比为3)为1.92 mg/L,在9.60～48.0 mg/L质量浓度范围内有良好的线性关系(r=0.995),迁移时间的相对标准偏差(RSD)为2.7%。将该方法用于硫酸沙丁胺醇片和硫酸沙丁胺醇气雾剂中的硫酸沙丁胺醇含量的测定,加标回收率为90%～113%,检测结果与药厂的标示值相符合,为硫酸沙丁胺醇的检测提供了一种简便、快速、高灵敏的方法。关键词: 毛细管电泳;非接触电导检测法;硫酸沙丁胺醇;硫酸沙丁胺醇片;硫酸沙丁胺醇气雾剂     

反相高效液相色谱法测定妇炎消片中盐酸小檗碱含量

反相高效液相色谱法测定妇炎消片中盐酸小檗碱含量;炎消片;盐酸小檗碱;高效液相色谱法     

反相高效液相色谱法测定野生与栽培花锚药材及其制剂中的花锚甙和去甲氧基花锚甙

建立了花锚药材及其制剂中两种抗肝炎有效成分花锚甙和去甲氧基花锚甙的反相高效液相色谱测定方法。采用甲醇回流提取进行样品处理,在乙腈 磷酸水溶液为流动相作梯度洗脱、ODS柱、检测波长为254 nm条件下,花锚甙和去甲氧基花锚甙均可达到基线分离。两种成分在0.68～3.40 g/L ,0.36～1.8 g/L 时,其峰面积与浓度成良好的线性关系,加标回收率为95%～105%。该法适用于花锚药材及其制剂的质量分析检验。     

三波长融合指纹图谱结合6组分定量和主成分分析评价银翘解毒片的质量

建立了三波长融合高效液相色谱指纹图谱,并结合6组分定量和主成分分析(PCA)评价25批银翘解毒片的质量一致性。采用反相高效液相色谱法(RP-HPLC)分别于230、279、327 nm下检测。运用多波长融合指纹图谱技术建立银翘解毒片三波长融合指纹图谱,采用系统指纹定量法对其进行定性和整体定量评价。结果鉴别出25批银翘解毒片样品完全合格且区分良好。同时测定6组分含量,与指纹图谱结合,从整体和局部角度评价银翘解毒片质量。此外,运用PCA法对融合指纹图谱进行分析,通过主成分得分图可以明显区分来自两个厂家的25批银翘解毒片样品。方法综合性较强且有效,为科学评价与有效控制银翘解毒片的质量提供了可靠的参考。     

Validated Method for Tadalafil Analysis in Pharmaceutical Preparations by Capillary Electrophoresis

A simple, rapid and inexpensive capillary electrophoretic method has been developed and validated for the determination of tadalafil in pharmaceutical preparations. The analysis was carried out using a fused silica capillary (60 cm × 75 m I.D.), phosphate buffer (50 mM, 3.0 pH) as back ground electrolyte (BGE), 15 kV applied voltage with UV detection at 254 nm and at a working temperature of 23 ± 1 °C. Linearity was observed in the concentration range from 200–5000 g/mL, with a correlation coefficient (R²) of 0.9998 and 200 g/mL as the limit of detection. The percentage recovery of tadalafil from pharmaceutical preparations was 99.5. Validation parameters prove the precision of the method and its applicability for the determination of tadalafil in pharmaceutical tablet formulations. The method is fast and is suitable for high throughput analysis of the drug.