Objective:To study stability of 9-nitrocamptothecin(9-NC)under the influence of stress testing,ac- celerated testing and long-term testing.Method:By observing change of 9-NC compared with control sample by HPLC.9-NC and its related substances were separated and determined on Eclipse~XDB-C_(18)(4.6 mm×150 mm,5 μm)column with mobile phase of acetonitrile-water(28.5:71.5)and a flow rate of 1.0 mL·min~(-1)at 25 ℃ with the UV detection at 368 nm.Results:9-NC was easy to change due to light and was relatively stable due to temperature,humidity,accelerated testing and long-term testing.Conclusion:9-NC should be stored away from light to keep its stable.

AIM:To establish the high performance liquid chromatography(HPLC)for determining 9- nitrocamptothecin(9-NC)and its related substances.METHODS:The HPLC was performed on Eclipse~(?) XDB-C18(5μm,4.6mm×150mm)column.The mobile phase consisted of acetonitrile and water(28.5:71.5, V/V).The flow rate was 1.0mL·min~(-1).The detection wavelength was set at 368nm.RESULTS:The assay showed good linear correlation over the range of 0.005-0.3g·L~(-1)(r=0.999 98).The minimum detection limit of 9-NC was 0.17ng.The average recovery rate of this method was 100.4%.The sample solution was stable within 3h.The coefficient variations of intra-and inter-day of 9-NC were less than 1.6%.The concentrations of three samples of 9-NC were 99.94%,99.31%,98.88%,and the related substances in 9-NC were 0.24%, 0.23%,and 0.28%,respectively.CONCLUSION:The HPLC is simple,sensitive,and accurate in the application to the quality control of 9-NC.

Objective:To establish HPLC method for the determination of content and related substance of rahit- rexed.Method:A Diamonsil C_(18)(4.6 mm×150 mm,5μm)column was used.The mobile phase was composed of buffer(0.03 mol·L~(-1) K_2 HPO_4-0.03 mol·L~(-1)(CH_3 CH_2)_3 N,pH=7.2 )-CH_3 OH (69:31).Detection wave- length was 342 nm.Flow rate was 0.9 mL·min~(-1).The temperature of the column was 35℃.Results:The linearity of the calibration curve was well correlated(r=0.9997) within the range of 1.0-100.0 μg·mL~(-1).The recovery was 99.94%-102.16%.The within and between day RSD were less than 2.22%.The content of related sub- stances were less than 0.58%.Conclusion:The method is simple,rapid,results are accurate and good reproduci- ble.The content and related substance of raltitrexed are both within acceptable range.

Purpose To determine the contents of residual methanol, ethanol,acetone, aether, petroleum ether, ethylacetate, iodomethane, acetic acid, n-amylamine,diethyl oxalate and DMF in Tegaserod Maleate. Methods A simple capillary gas chromatography method was established with FID detector. The capillary column was HP-5, using temperature program; The residues were calculated by the external standard method. Results The linearities were fairly good. The average recoveries were 86. 87 % - 98. 45 % with RSD of 1. 34% - 6. 56%. The limit of detection was 0. 29 - 1. 06 ng. The contents of eleven residual organic solvents in four batches of samples were complied with the specification requirements. Conclusions After validation, the method was proved to be accurate,sensitive and reliable. It is suitable to be adopted in the analysis of the tested solvents.

Objective:An HPLC method was established to determine the content and the related substances of tegas-erod maleate tablets,and then its stability was studied with this method. Method:Agilent HPLC instrument was used with the column:Diamonsil C18150 mm×4.6 mm (5μm). The mobile phase was acetonitrile - 1% sodium dodecyl sulfate(contain 0.95% acetic acid) (56:44) ;the wavelength of the UV absorbance detector was 314 nm;the flow rate was 1 mL· min-1 (for determination of related impurities)or 2 mL· min-1 (for determination of tegaserod maleate content)and the column was maintained at 40℃. Results:The standard curve was linear in the range of 0.0001 -0.12 mg·mL-1 and the linear equation was A = 28.93C -14.46(r =0.9999,n =6). The within -day precision wasless than 1.1% (RSD) ,and the between -day precision was less than 3. 1% (RSD). The average recovery was between 100.4% -103. 8%. Conclusion:The HPLC method is specific,sensitive and reliable. The results of the stability study of tegaserod maleate tablets verify that the tablets should be stored in a dry and cold condition.

AIM:To establish a reversed-phase HPLC method with fluorescence detection for determination of the concentration of propofol in human plasma. METHODS: Agilent 1100 HPLC instrument was used with the column : Diamonsil C 18(150 mm×4.6 mm,5 μm), Phenomenex Security Guard column(4 mm×3 mm). Plasma samples were precipitated with the thymol (internal standard) methanol solution. 20 μL of supernatant fluid was injected for HPLC analysis. The mobile phase was composed of acetonitrile-water(56:44,V/V).The flow rate was 1.5 mL·min -1. The fluorescence detective wavelengths were: λ ex=276 nm, λ em=312 nm. RESULTS: The standard curve equation was Y= 1.787C- 0.031 (r= 0.9997,n=9).The linear range was (0.02—8.0) mg·L -1. The average recovery was 98.71 %.Intra- and inter-day precision(RSD%) were all less than 4.2 %. The limit of detection was 4 μg·L -1(S/N=2). CONCLUSION:The RP-HPLC method is simple, sensitive and accurate for monitoring propofol concentration in clinical plasma samples.

目的:建立反相高压液相色谱法测定亚叶酸钙片剂和胶囊含量的方法,同时检查其有关物质,并进行稳定性考察.方法:采用Lichrosorb C18色谱柱,以乙腈∶10 mmol*L-1醋酸钠-三乙胺缓冲液(冰醋酸调pH至5.5)(4∶96)为流动相,流速1.2 mL*min-1;检测波长286 nm,柱温为常温.结果:在色谱条件下,亚叶酸钙制剂的分析不受辅料和降解产物的干扰,其检测限为0.04 μg,定量限为0.12 μg,在12.5～150 mg*L-1范围内线性关系良好(r=0.9998),加样回收率为99%～101%,日内、日间RSD<3.0%.结论:本法灵敏准确,方便实用.

AIM: To establish UV and HPLC methods to determine the content of tegaserod tablet. METHODS: HPLC method——the separations were obtained on a Diamonsil C18 column which was maintained at 40 ℃, the mobile phase was acetonitrile 1% sodium dodecyl sulfate (contain 0.95% acetic acid) (56∶44, V∶V), the flow rate was 2 mL·min -1 and the detection wavelength was 314 nm. UV method——absorption was determined at 314 nm. RESULTS: HPLC method——calibration was linear from 0.1-120 mg·L -1 ( r =0.9999). Within day and between day coefficients of variation were less than 3.1 % . The recovery was between 100.42 % - 103.82 % . UV method——calibration was linear from 2-20mg·L -1 ( r =0.9998). Within day and between day coefficients of variation were less than 1%. The recovery was between 101.06 %-103.02 %. CONCLUSION: HPLC and UV method both appear to be suitable for determination of the content of tegaserod tablet while we are apt to use the UV method for its simplicity if the related impurity is controlled well.

AIM: To compare the pharmacokinetic parameters of the two kinds of omeprazole capsules, following per oral administration. METHODS: Twenty healthy volunteers were per orally cross-administrated two kinds of omeprazole two capsules (20 mg omeprazole per capsule). The plasma concentrations of omeprazole were determined by the reverse phase high performance liquid chromatography (RP-HPLC) method. The pharmacokinetic parameters of two capsules preparations were calculated and compared by 3P97 Software. RESULTS: The concentration-time curve of omeprazole complied with the single compartment model. Following per oral administration of omeprazole 40 mg, there were no statistical significant differences of the main pharmacokinetic parameters between the two capsules preparations by the analysis of variance (P0.05). The relative biological availabilities of the two capsules preparations were (95.5-110.7) %. CONCLUSION: The results demonstrate that the two kinds of omeprazole capsules are bioequivalent.

AIM: To evaluate the quality of three marketed isosorbide nitrate intravenous injections. (Isosorbide dinitrate from Zhuhai Schwarz Pharma.,Shandong Qilu Pharma., and isosorbide mononitrate from Shandong Lunan Pharma.) METHODS: HPLC, GC, and freezing point depression methods were used to examine the qualities of three isosorbide nitrate intravenous injections. RESULTS:While few differences existed in the assays of the three brands, there was great difference in osmolarities of three products:the product from Zhuhai Schwarz Pharma.was isotonic (289 mmol·L -1 ), but the other two products were both hyperosmotic (2000 mmol·L -1 ). After analysis by HPLC and GC MS, 1,2 propanediol was found to exist in both injections at concentrations ranged from 23 % to 28 % (kg·L -1 ), and 17 % to 23 % (kg·L -1 ), which led to an abnormal high osmolarity. CONCLUSION:It indicate that all three brands are confirmed with their own product standards, but great difference exists in osmotic pressures of three products, due to 1,2 propanediol containing in two of three products.

AIM:To establish a reversed-phase high pressure liquid chromatography(HPLC) method to determine the concentration of clindamycin phosphate and to investigate the stability of its injections. METHODS: Lichrosorb C 18 colum (150 mm × 4.6 mm, 5 μm )was used with the mobile phase of triethylamine chlorhydric acid solution (30mmol·L -1 ,pH=2.65)∶acetonitrile being 80∶20(V/V),flow rate of 1.0 mL·min -1 and detection wave lenth of 210 nm. RESULTS: The standard curve equation was y =597075c-62541.8( r =0.9997, n =5).The linear range was 0.4 - 1.6g·L -1 . The average recovery rate was 98.9 %.The intra day and inter day precision rate were less than 5 %.There was no difference between four products from different factories with respect to their stabilities to the light, whereas there was a few difference between the sample 1,4, and sample 2, 3, with respect to their stabilities to the heat. CONCLUSION: The RP-HPLC method was simple, rapid and sensitive. The clindamycin phosphate injection is stabilized to the light, but not stabilized to the heat.

目的:建立测定盐酸曲马多血药浓度的反相高效液相色谱分析法,并测定该药的临床稳态血药浓度.方法:色谱柱:Lichrosorb C18(150 mm×4.6 mm, 5 μm).在1.0 ml血样中加入内标非那西丁后,以7.0 ml乙醚一次提取,进行色谱分析.流动相为醋酸钠缓冲液(50 mmol/L, pH 3.5)-乙腈=75∶25(V/V),流速1.0 ml/min,检测波长271 nm.结果:线性方程为Y=0.921 5c-0.146 5(r=0.999 0, n=7),线性浓度为0.2～3.0 μg/ml,最低检测浓度为0.1 μg/ml血浆(信噪比=2),平均方法回收率为102.35%,日内、日间RSD均＜5%.测得盐酸曲马多稳态血药浓度为(0.521±0.216) μg/ml.结论:本方法简便、准确、灵敏,可用于测定盐酸曲马多在人血浆中的药物浓度,为临床研究提供可行的分析方法.