目的:建立顶空气相色谱法测定安立生坦原料中甲醇、乙醇、叔丁基甲基醚、乙酸乙酯、二氧六环、N,N-二甲基甲酰胺等残留量的方法.方法:采用HP-5(30 m ×0.53 mm,1.5 μm)石英毛细管柱,载气为高纯氮气,FID检测器,采用程序升温和顶空进样,柱温35℃保持5min,再以20℃·min-1升温至110℃,保持5min.结果:6种残留溶剂的分离度符合要求,线性关系良好(r≥0.999 0).回收率均在99.3％～105.2％范围内,3批安立生坦样品检测结果均符合限度要求.结论:该方法检测灵敏、准确,可用于检测安立生坦原料药的残留溶剂.

目的 筛选安立生坦片的最佳处方.方法 通过原料辅料的相容性试验筛选辅料,采用正交试验考察不同处方对颗粒流动性、外观、溶出度的影响,确定最优处方,与市售安立生坦片在4种溶出介质中进行累积溶出曲线对比研究,并考察制剂的加速稳定性.结果 开发出最优处方,产品与市售安立生坦片在4种溶出介质中溶出曲线相似,6个月的加速试验结果与0个月时比较无明显变化.结论 该处方设计合理、制备工艺可靠.

Objective To establish a method for determination of related substances in ambrisentan active pharmaceutical ingredients. Methods HPLC method was adopted. The determination was performed on Waters Atlantis T3 column (250 mm × 4.6 mm, 5μm) with mobile phase consisted of 0.02% trifluoroacetic acid - acetonitrile (containing 0.01% trifluoroacetic acid) with gradient elution. The temperature of column was set at 30℃. The flow rate was 1.0 mL/min with automatic injection volume of 5μL. The detective wavelength was set at 220 nm. Results Ambrisentan and its related substances could be separated completely. The LOQ of the related substances, such as Z1, Z2, Z3, Z4, and DP1 were 2.14, 2.54, 2.44, 2.45, and 2.41 ng, respectively. They all had good linearity. The average recovery were 102.9%, 96.0%, 93.1%, 104.6%, and 115.2%with RSD values of 2.1%, 4.6%, 2.9%, 2.7%, and 4.9%(n = 10), respectively. Conclusion The method is sensitive and accurate, and can be used for quality control of related substances in ambrisentan active pharmaceutical ingredients.

Objective:To develop a method for the quantitative determination of ambrisentan. Methods: 1 H NMR spectra were obtalned with a Bruker AscendTM 400 superconducting NMR spectrometer. For each sample, DMSO-D6 was used as the solvent, the pulse width was 10. 0 μs, the delay time was 5 s and the scanning time was 16. Results: The proton peaks of ambrisentan at δ6. 16 ppm and maleic acid atδ6. 28 ppm were used as the quantitative peaks. The linear regression equation of peak area and quality ratio was Y=0. 140 7X+0. 034 8 with the correlation coefficient of 0. 999 4. RSD was 0. 2%(n=6)in the repeated experiments. The absolute content of ambrisentan reference substance was 99. 9%. Conclusion: The results showed that 1 H NMR can be used in the quantitative determination of ambrisentan without reference substance. The method is reliable, rapid, accurate and simple.

Objective To establish an HPLC method for determining fenofibrate in Fenofibrate Sustained-release Tablets. Methods HPLC was carried out on a Dikma C18 column(200 mm × 4.6 mm, 5 μm) with methanol- water(90∶10) as mobile phase. The detection wavelength was set at 288 nm. The injection volume was 20 μL at the flow rate of 1.0 mL/min. The temperature of column was set at 25 ℃. Results There were good linear relationship of fenofibrate in the range of 2 — 12 μg/mL(r = 0.999 9). The limits of detection and quantitation were 10 and 30 ng/mL, respectively. The average recoveries was 99.86% with RSD value of 0.72%(n = 9). Conclusion The method is accurate and simple for quality control of fenofibrate in Fenofibrate Sustained-release Tablets.

This study was aimed to identify the main related substance in baicalein in order to provide basic study data for the safety, efficacy and quality control of the medicine. The analysis was carried out on activated carbon and silica gel column. The compound structure was identified by spectral analysis, which included UV, IR, NMR and MS. The results showed that the related substance was identified as oroxylin A. It was concluded that the determina-tion provided scientific data for studying the impurities of baicalein and improving its quality.

This study was aimed to establish a HPLC fingerprint of saponins in Sanjie-zhentong Capsule in order to make a quantitative analysis of the quality of Sanjie-zhentong Capsule. The Waters Symmetry ShieldTM RP18 (4.6 mmí 250 mm, 5 μm) column was used with a mobile phase of acetonitrile-water gradient elution. The flow rate was 1.2 mL/min. The column temperature was 30℃. The detection wavelength was 203 nm. The results showed that the fingerprint chromatography included 9 mutual peaks. The similarity among batches was more than 0.95. Compared with reference substance, five characteristic components were recognized. The five components are notoginsenoside R1, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1 and ginsenoside Rd. It was concluded that this method was rapid, simple and accurate and can be used as one of the effective methods for the quality control of Sanjie-zhen-tong Capsule.

目的:建立测定盐酸决奈达隆片含量及有关物质的方法。方法:采用高效液相色谱法。色谱柱为C18,以甲醇-乙腈-磷酸盐缓冲溶液（32∶50∶18）为流动相,流速为1.5 ml/min,检测波长为220 nm,柱温为40℃。结果:决奈达隆与各杂质分离度良好,盐酸决奈达隆检测质量浓度线性范围为5.2~103.0μg/m（lr=0.999 9）,低、中、高质量浓度回收率分别为100.4%、100.6%、100.2%,平均回收率为100.4%,RSD=0.8%（n=3）;杂质A、杂质B、主成分、杂质C、杂质D的检测限分别是0.25、0.25、0.5、1.0、1.0 ng。结论:建立的方法专属性好、操作简便,可用于盐酸决奈达隆片含量及其有关物质的测定。

Objective:To establish an HPLC method for the determination of the content and related substances of lapatinib ditosylate.Method;The HPLC analysis was performed on an ODS column(250 mm×4.6 mm,5 μm) with a mobile phase of acetonitrile-0.005 mol · L~(-1) ammonium acetate solution(55:45) at the flow rate of 1.0 ml · min~(-1).The UV detection wavelength was 260 nm.The column temperature was at 30℃ and the sample size was 20 pi.Result:Good chromatographic separation of lapatinib and its related substances were obtained.The calibration curve was linear within the range of 10.4-207.2 ag · ml~(-1)(r =0.999 9) for lapatinib ditosylate.The detection limit was 0.5 ng.Conclusion;The method is convenient and specific,and can be used in the determination of the content and related substances of lapatinib ditosylate.

目的考察藤黄酸在高温、高湿、强光照、氧化、稀碱水溶液及不同有机溶剂中的稳定性。方法采用高效液相色谱法测定供试品中藤黄酸的量。结果藤黄酸在稀氢氧化钠溶液、高温、乙醇等有机溶剂中不稳定;在强光照、高湿及氧化条件下较稳定。结论藤黄酸对热较敏感,在稀碱溶液、乙醇中不稳定,制剂研究要考虑避免高温及接触碱性溶液、乙醇。

OBJECTIVE:To establish the chromatographic fingerprint for the quality control of gamboge.METHOD:Analysis on a Luna C8 (4.6 mm x 250 mm, 5 microm) column eluted with mobile phases containing acetonitrile and 0.1% glacial acetic acid in water in gradient mode. The flow rate was 1.0 mL x min(-1) and the detection wavelength was at 362 nm. The temperature of column was 25 degrees C. And data of 11 batches of gamboge samples from different sources were analysed by "similarity evaluation for chromatographic Fingerprint of Traditional Chinese Medicine" software.RESULT:Thirteen common peaks were selected in chromatograms, and all the common peeks were separated effectively.CONCLUSION:The precision, repeatability, and stability of this method were satisfying. The method developed can be used to identify and evaluate the quality of gamboge.

目的:建立利胆溶石软胶囊的指纹图谱,更有效地控制该产品的质量。方法:采用GC法HP-5毛细管色谱柱,进样温度240°C,检测器温度240°C,分流比,50∶1,程序升温,载气流速1.5 mL/min。结果:测定了原料的指纹图谱,以薄荷脑(7号峰)为参照进行了测定,共有10个色谱峰,香葵油原料以香叶醇(8号峰)为参照进行测定,共有5个色谱峰,并标示出利胆溶石软胶囊共有峰,并对各共有峰进行初步归属判断。结论:该方法为利胆溶石软胶囊的质量控制提供了较全面的信息,利于产品的质量控制。