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The development and validation of an isocratic high performance liquid chromatographic method is de-scribed for the determination of tamsulosin hydrochloride in sustained release tablets. The determination was per-formed on a Diamonsil BDS C18 column with a mobile phase consisting of a mixture of acetonitrile, methanol and 0.5% phosphoric acid solution (20:30:50, V/V/V) at a flow rate of 1.0 mL/min. UV detection was made at 274 nm. The linear range for tamsulosin hydrochloride was 0.81 - 8.10μg/mL. The mean recovery was 99.8%(SR = 0.7 %, n = 9), and the precision was found to be 0.45 % ( n = 9). The proposed method can be used for routine analysis of tamsulosin hydrochloride in sustained release tablets. 相似文献
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An isocratic reversed-phase liquid chromatographic (LC) method is described for the determination of epalrestat and its three stereoisomers (degradation impurities) in drug substance. The LC separation system consisted of a Hypersil C18 column (250 mm×4.6 mm, 5 μm) with a mobile phase comprising methanol, acetonitrile and water (volume ratio 60∶1∶50, pH 4.5) delivered at a flow rate of 1.6 mL/min and UV detection at 280 nm. The proposed LC method is simple and selective for the determination of the stereoisomers of epalrestat in the drug substance with a limit of detection and quantification of 3.9 μg/mL and 4.9 μg/mL, respectively. The stereoisomers were identified by liquid chromatography-mass spectrometry (LC-MS). 相似文献
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New cyclodextrin derivatives(CDs),heptakis(2,6-di-O-methyl-3-O-methoxymethyl)-β-CD(Ⅰ)and heptakis(2,3,6-tri-O-methoxymethyl)-β-CD(Ⅱ),were investigated for their chromatographic performance as stationary phases for capillary gas chromatography(CGC).Both of the CDs exhibited good selectivity and satisfactory separation for test mixtures and aromatic positional isomers,and volatile compounds from Ligusticum chuanxiong Hort.Additionally,the selectivity and elution orders of major compounds were compared with a ... 相似文献
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建立了固相萃取-气相色谱-串联质谱法(SPE-GC-MS/MS)同时测定木制儿童用品中氯酚类化合物和菊酯类化合物等10种木材防腐剂。采用甲醇溶剂提取,乙酸酐试剂衍生、固相萃取净化后,经HP-5MS色谱柱(30 m×0.25 mm×0.25 μm)分离,串联质谱在多反应离子监测模式(MRM)下进行检测,内标法定量。同时,考察了多种实验参数对检测结果的影响,并进行方法验证。结果表明,该方法对于复杂基质的木材样品中目标物的检测具有良好的选择性与灵敏度。对于不同物质的定量限(LOQ)在0.002 5~0.2 mg/kg之间,线性范围为0.002 5~25 mg/kg,低、中、高3个添加水平的平均回收率在85.2%~100.1%之间,日内精密度(RSD,n=6)在0.6%~9.1%之间,日间精密度(RSD,n=6)在2.3%~7.2%之间。将该方法应用于实际样品抽查中,发现了多种木材防腐剂的残留。 相似文献
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建立了一种HPLC法,用于制剂中盐酸噻氯吡啶和尼群地平的含量测定,并就方法的选择性、准确性、精密度、检测限和定量限等对方法进行了认证.采用C18色谱柱,以乙腈-甲醇-醋酸铵(60∶10∶30 (V/V), pH 6.5)为流动相,流速为1.0 mL/min,检测波长为236 nm.盐酸噻氯吡啶和尼群地平含量测定的线性范围为75~750 μg/mL (R=0.999 9,n=5)和1~10 μg/mL (R=0.999 9,n=5);平均回收率分别为100.1(SR=0.6%,n=9)和99.9(SR=0.7%,n=9);日内精密度分别为0.63%和0.74%,日间精密度分别为0.89%和1.00%.本法快速、准确、选择性高,可用于药物制剂中盐酸噻氯吡啶和尼群地平的同时测定. 相似文献
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利用在线监测系统测定了光卤石中氯化钾的溶解度,并采用Van′t Hoff方程对其溶解度数据进行拟合。探讨了不同类型的表面活性剂及其含量对光卤石中氯化钾结晶介稳区宽度的影响以及在不同过饱和度下表面活性剂对诱导期的影响,并结合诱导期数据计算了固-液界面张力γ值。结果表明:Van′t Hoff方程能够对氯化钾溶解度很好地拟合;3种不同类型的表面活性剂都使介稳区宽度变宽;加入阴、阳离子表面活性剂,随着其含量的增大介稳区变宽,而加入非离子表面活性剂,其含量对介稳区宽度的影响不大。在恒定温度下,随着过饱和度增大,结晶诱导期时间变短,而加入表面活性剂使诱导期时间变长。 相似文献