目的 建立HPLC梯度洗脱法测定利福霉素钠及注射用利福霉素钠的有关物质.方法 选用Waters C18色谱柱,以0.18％磷酸二氢钠溶液(用8.5％的氢氧化钠溶液调解pH值至7.5)-乙腈(90:10)为流动相A;0.18％磷酸二氢钠溶液(用8.5％的氢氧化钠溶液调解pH值至7.5)-乙腈(50:50)为流动相B;梯度洗脱[0min(70％A)→35min(15％A) →37min(70％A) →47min(70％A)];流速为1 mL/min,检测波长为254nm.结果 经过方法学验证试验,认定方法可行.结论 本方法灵敏、准确,专属性强.

目的:完善利福霉素钠制剂的无菌检查方法.方法:采用薄膜过滤,选用组氨酸-卵磷脂-聚山梨酯80混合溶液作为冲洗液进行无菌检查.结果:此法能有效消除抑菌成分的干扰,各试验菌生长良好.结论:经过方法学验证,所建立的方法适用于注射用利福霉素钠及利福霉素钠注射液的无菌检查.

Objective To establish a determination method for five residual solvents in Rifamycin sodium.Methods DB-5 capillary column was adopted with inlets temperature at 200 ℃;FID detector and programmable temperature was applied.The initial temperature was 40 ℃ and kept for 8 min,the temperature was then raised to 200 ℃ at the rate of 15 ℃·min-1 and lasted 2 min.Results Five residual solvents were completely separated with good linear relationships(r=0.9933-0.9999).The average recovery rates were in the range of 82.0%-102.0%(RSD=1.2%-5.3%,n=9).Conclusion The methods was proved to be accurate and sensitive,which can be used for the determination of residual solvents in Rifamycin sodium.

Objective To establish a HPLC method for the determination of cefoperazone impurity C in cefoperazone sodium and sulbactam sodium for injection.Methods The analytes were analyzed on a C_(18) column, using a mixture of 0.005mol/L tetrabutylammonium hydroxide solution-acetonitrile(75:25) as the mobile phase with a flow rate of l.0mL/min.Detection wavelength was 220nm,and the column temperature was maintained at 30℃. Results Cefoperazone impurity C was well separated from other impurities and both of cefoperazone and sulbactam were completely separated from their related substances.The calibration curve was linear in the range of 3.19~25.6μg/mL and the correlation coefficient was 0.9998.The average recovery was 97.45%and the RSD was 2.4%(n=9).Conclusion The established method is accurate,sensitive and specific.It is suitable to determinate cefoperazone impurity C in cefoperazone sodium and sulbactam sodium for injection and can be effectively used for quality control of the drug.

An HPLC method was established for the determination of the related substances of antituberculosis fixed-dose combination(FDC)of rifampin,isoniazid and pyrazinamide.A C18 column was used with the mobile phase of 0.01 mol/L phosphate buffer-methanol(40︰60) at the detection wavelength of 254 nm.The results of specificity test,system suitability test,durability test and solution stability test showed that the proposed method was feasible.The determination of related substances is beneficial to the quality control of compound drugs.

目的 建立利福喷丁胶囊微生物限度检查方法.方法 分别采用常规法、离心集菌法、离心集菌+薄膜过滤法对样品进行微生物限度检查,根据5株阳性菌的回收率结果进行数理统计.结果 试验结果表明,利福喷丁胶囊具有较强的抑菌活性,离心沉淀集菌+薄膜过滤法能有效的去除其抑菌性.结论 用该法进行微生物限度检查,可以客观的反映药品中微生物的污染状况,可行性强,能达到检验目的 .

Objective To perfect the method for determination of related substances of Rifamycin Sodium Injection.Methods A HPLC method with graduate elution was applied,equipped with Waters ODS C18 column,using acetonitrile-0.39% solution of sodium dehydrogenate phosphate(adjusted to pH 7.5 with dilute sodium hydroxide solution)(10∶90)as mobile phase A and acetonitrile-0.39% solution of sodium dehydrogenate phosphate(adjusted to pH 7.5 with dilute sodium hydroxide solution)(70∶30)as mobile phase B.Graduate elution:For 0~40 minutes,the proportion of mobile phase B increased linearly from 20% to 80%.After hold on for 5 minutes,within 2 minutes the proportion of mobile phase B decreased linearly from 80% to 20%.Then hold on for 8 minutes.Flow rate was 1.0mL·min-1 and detective wavelength was 254nm.Results After specificity experiment,quantitative limits experiment,durability experiment and liquid stability experiment,the method is proved to be feasible.Conclusions The revised quality standard has obvious improvement in efficacy and controllability.It is practicable to apply the method for determination of related substances of Rifamycin Sodium Injection.

Objective To establish a methods for determining sterility test of Cefonicidum Natricum for Injection.Methods The membrane filtrating and enzyme methods were used.Results It had higher antimicrobial effects.There were dramatically different antibacterial sensitivities to the validating bacteria among the generations of cefonicidum natricum due to their different antibiotics profiles.Conclutions Membrane filtrating and enzyme methods have higher antimicrobial effect,meanwhile the validity of sterility test for the Cefonicidum Natricum for Injections is assured.

The suggestion was presented about addition of dissolution determination of isoniazid and pyrazinamide in isoniazid,rifampin and pyrazinamide compound capsules and compound tablets.An UV method was established for determination of rifampin,and an HPLC method was established for determination of isoniazid and pyrazinamide.The calibration curves of rifampin,isoniazid and pyrazinamide were linear in the concentration ranges of 16-40μg/ml,12.2-30.8μg/ml and 38.7-117μg/ml.The average recoveries were 99.4%-100.4%,RSDs were less than 0.55%.

氢溴酸右美沙芬属人工合成的吗啡衍生物--吗啡南类非成瘾性中枢镇咳药,其镇咳作用与可待因相仿,但无镇痛作用,适用于感冒、急慢性支气管炎、咽喉炎、肺结核及其他上呼吸道感染引起的咳嗽[1].本文考察氢溴酸右美沙芬在不同条件下的稳定性,为制定储存条件及有效期提供依据.

Objective:To establish a method for assay determination of Dextromethorphan Hydrobromide and Guaifenesin for Suspension.Methods:An HPLC method with graduate elution was applied,equipped with Diamonsil C_(18) column(4.6mm×15cm),using 0.075mol·L~(-1)triethylamine phosphate(pH2.8±0.2)-acetonitrile(75:25).Flow rate was 1.0ml/min and de- tective wavelength 280nm.Results:The linear ranges of Hydrobromide and Guaifenesin,and Dextromethorphan were 25.0～125.0μg·ml~(-1),167.6～838.2μg·ml~(-1),and the recoveries of Dextromethorphan Hydrobromide and Guaifenesin for Suspen- sion were 100.6%(RSD=0.81%),99.4%(RSD=0.46%),respectively.Conclusion:The method is accurate,sensitive,an- d reliable.It is practicable to apply the method for the assay of Dextromethorphan Hydrobromide and Guaifenesin for Suspension.

Objective:To establish a method for determination of assay of Rifampin,Isoniazid,and Pyrazinamide Capsules and Tablets. Methods:An HPLC method with graduate elution was applied,equipped with Kromasil ODS C_(18) column(5μm,4.6mm×20cm),using acetonitrile-0.05mol/L ammonium dihydric phosphate(3∶97)as mobile phase A and acetonitrile-0.05mol/L ammonium dihydric phosphate(55∶45)as mobile phase B.After isocratic elution with mobile phase A for 4 minutes,the proportion of mobile phase B increased linearly from 0% to 100% within 4 minutes and then hold on for 7 minutes.Flow rate was 1.0ml/min and detection wavelength 263nm.Results:The linear ranges of Rifampin,Isoniazid,and Pyrazinamide were respectively between 20.1-100.5μg/ml,13.5-67.3μg/ml,66.6-333.2μg/ml,and the recoveries of Rifampin,Isoniazid,and Pyrazinamide in Compound Capsule were 99.8%(RSD=0.44%),99.1%(RSD=0.24%),100.5%(RSD=0.40%),respectively;and the recoveries of Rifampin,Isoniazid,and Pyrazinamide in Compound Tablet were 100.1%(RSD=0.12%),100.3%(RSD=0.53%),100.4%(RSD=0.35%),respectively.Conclusion:The method is accurate,sensitive,and reliable.It is practicable to apply the method for the assay of compound capsule and tablet.

头孢他美(Cefetamet)系以7-ADCA为原料而合成的新的头孢类抗生素.据有关文献报道,该药对革兰氏阳性菌及革兰氏阴性菌的抗菌活力与头孢克肟,头孢噻肟相当,对淋球菌、布兰汉氏菌、大肠杆菌、肺炎杆菌、肠杆菌属、变形菌、普罗威登斯菌属等革兰氏阴性菌的抗菌活性优于阿莫西林、头孢克罗和头孢孟多.本品对需氧菌,厌氧菌所产生的青霉素酶,头孢菌素酶,氧亚氨头孢菌素酶等多种β-内酰胺酶稳定.本文筛选以头孢氨苄,头孢噻肟为对照药,试验了该三种原料药对218株临床分离菌株的体外抗菌作用,质控菌为ATCC26006.

Objective To Study the stability of doxycycline hyclate dispersible tablets. Methods The characteristics , relate substances, assay of doxycycline hyclate dispersible tablets were measured after the samples tested under high temperature, high humidity and light radiation for 10 days; 40℃,75% humidity for six months; laid in the air in two years. Results Under the testing conditions, no obvious changes were observed. Conclusion Doxycycline Hyclate Dispersible Tablets shows good stability.

目的建立注射用法罗培南钠的含量测定方法.方法采用高效液相色谱法,选用ODS C18色谱柱(4.6 mm×150 mm),流动相:以磷酸盐溶液(取磷酸二氢钾4.8 g,磷酸氢二钠5.4 g和四丁基溴化铵2.0 g,加水溶解使成1 000mL)-乙腈-甲醇(70:10:20);流速:1.0 mL·min-1,检测波长:230 nm.结果法罗培南钠在0.102 0～0.815 7 g·L-1的浓度范围内,面积与浓度呈良好的线性关系.回收率为100.1%,RSD为0.20%.结论方法准确、灵敏、可靠,适用于注射用法罗培南钠的含量测定.