目的:建立超高效液相色谱法同时测定复方斑蝥胶囊中马钱苷和紫丁香苷的含量.方法:以乙腈-水(8:92)为流动相;流速0.4mL/min;检测波长230nm.结果:马钱苷、紫丁香苷的线性范围分别为:2.1760~21.760、2.4980~24.980 μg/mL,相关系数r2均为0.9999;平均加样回收率为:101.2%、99.1%,RSD值为3.27%、1.7%.结论:本方法操作简单,重复性好,准确可靠,可用于复方斑蝥胶囊中马钱苷和紫丁香苷的含量测定.
为提高葫芦饮片的质量标准评价体系,为葫芦质量标准的制定及资源的开发利用提供依据,采用薄层色谱法对葫芦饮片进行定性分析,采用HPLC法测定莽草酸含量,并根据2020年版中国药典方法测定葫芦饮片水分、灰分.结果发现,葫芦饮片薄层色谱斑点均清晰明显,同时10批葫芦药材样品的水分为7.2%~9.4%,总灰分为3.8%~10.0%,莽草酸含量为0.002%~0.043%.
[目的]建立凤仙花药材中槲皮素、山奈酚的提取方法,对凤仙花药材中槲皮素、山奈酚进行薄层鉴别.[方法]采用羧甲基纤维素钠硅胶G板分离凤仙花药材中槲皮素、山奈酚成分.[结果]供试品色谱在与对照品色谱相应位置上显相同颜色的斑点,可用于鉴别凤仙花中的槲皮素和山奈酚.[结论]薄层色谱方法简便、专属性强、重现性好,可用于凤仙花药材的鉴别.
目的:建立同时高效液相色谱法同时测定凤仙花中槲皮素、山奈酚的含量。方法色谱柱采用十八烷基硅烷键合硅胶为填充剂(150 mm ×4 u.6 mm,5μm)。甲醇0.4%磷酸溶液(50∶50);检测波长:360 nm。结果槲皮素在0.1000~4.9987μg范围内,回归方程为Y=5.608×107X+8.018×104,R2=0.9999;山奈酚在0.098~9.777μg范围内,Y=5.7267×107X +3.8767×104, R2=0.9998,回收率槲皮素为102.27%, RSD 为0.66%;山奈酚为104.16%,RSD为0.83%。结论本方法操作简便,测定结果准确,重复性好,可用于凤仙花中槲皮素、山奈酚的含量测定。
[Objective] The reference for the determinate of the nitrophenol isomers in well water provided through the research.[Method] The material from well water was pretreatment with Dual-Cloud Point Extraction and measured with Capillary Electrophoresis.[Results] In the optimum condition,which concentration of the surfactant Triton X-114 was 0.5%,the pH was 1.5,the adding amount of NaCl was 0.020 g/ml,meanwhile,the adding amount of 0.2 mol/L NaOH was 100 μl,the nitrophenol isomers in well water were tested with the method of Dual-Cloud Point Extraction and Capillary Electrophoresis at the temperature of 40 ℃ for 20 minutes.There was good linearity between O-nitrophenol and M-nitrophenol in the range of 0.000 2-0.005 0 mg/mL,the recovery of the technique reached 97% and the relative standard deviation was less than 5%.[Conclusion] The result from the technique was accurate and environment-friendship because the effect of the surfactant in the accumulation phase on the isolation of capillary electrophoresis was eliminated.
The main components in roseous liquid were analyzed qualitatively by GC-MS combination method.The results indicated that 6 organic compounds which had never been reported till now were separated from the extract of hawthorn kernel oil.
A method based on cloud point extraction was developed to determine benzoic acid in milk using high-performance liquid chromatography detection.The non-ionic surfactant Tween-20 was chosen as extraction solvent,the extraction parameters affecting extraction efficiency,such as concentrations of Tween-20 and(NH4)2SO4,equilibration temperature,equilibration time and pH were evaluated and optimized.The optimum CPE conditions were:3%(V/V)Tween-20,300g/L(NH4)2SO4,pH4,equilibration temperature 90℃ for 10min;chromatographic conditions were:mobile phase of ammonium acetate buffer-methanol 90:10(V/V),flow rate 1mL/min,the detection wave length 230nm.Under the above optimized conditions,the linearity of the calibration curve for benzoic acid was in the range of 0.2~2.0μg/mL,the limits of detection was 0.025μg/mL,the correlation coefficient was 0.9998.The recovery for the standard addition of the benzoic acid in the milk ranged from 98.90% to 100.16%,the relative standard deviations was in the range of 1.2%~2.5%.
A method of micellar electrokinetic chromatography capillary (MECC) has been established for separating polymyxins E1 and E2 in polymyxin E sulfate and determining the contents of E1 and E2. Several factors including the running voltage, the type of surfactant, concentrations of Brij-35 (polyoxyethylene glycol dodecyl ether), NaCl solution and acetonitrile, pH of phosphate were investigated. Under the optimum conditions (10 kV running voltage, phosphate buffer solution (0.01 mol/L, pH 4.1) containing 30 mmol/L Brij-35, 5% (v/v) acetonitrile, 0.167 mol/L NaCl), E1 and E2 were separated with the resolution of 1.94. The contents of E1 and E2 in polymyxin E sulfate were 67% and 32%, respectively. As an example, the relative standard deviations of the intra-assay and inter-assay of polymyxin E1 on the plate number and peak area were less than 5%. The method is simple, rapid, accurate, and reproducible.