盐酸尼非卡兰的有关物质及含量测定方法

 目的分别用HPLC和非水酸碱滴定法建立起盐酸尼非卡兰有关物质检查及含量测定的方法,为原料的质量控制提供有效的分析方法。方法采用岛津CLC-ODS(6mm×150mm,5μm)柱,流动相:乙腈-0.02mol·L^-1的磷酸二氢钾溶液(NaOH溶液调pH至5.0)=25∶75;检测波长:268nm;流速:1.0mL·min^-1;柱温:30℃。结果在选定的色谱条件下,盐酸尼非卡兰与7个有关物质分离完全;盐酸尼非卡兰在5～100mg·L^-1内,峰面积与浓度线性关系良好,r=0.9999;检测限为0.2ng。结论方法简便,准确,专属性强,可用于盐酸尼非卡兰的有关物质检查及含量测定。     

盐酸丁卡因注射液的稳定性研究

 目的研究盐酸丁卡因注射液的稳定性及贮存期。方法用HPLC测定盐酸丁卡因及分解声物对丁氨基苯甲酸的含量,将产品用加速实验法,经典恒温法和室温留样观察法进行实验。结果盐酸丁卡因的含量随温度升高和时间延长逐渐下降,产品加速实验得出：温度40℃,湿度75%条件下,盐酸丁卡因放置1个月含量为98.68%,2个月为96.33%,3个月为94.37%。经典恒温法测得25℃的贮存期为15个月。室温留样观察实验证实：盐酸丁卡因注射液放置1年含量为96.67%,放置2年为89.34%。结论3种实验方法测得的数据基本一致。盐酸丁卡因注射液的有效期可暂定为1年。     

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??OBJECTIVE To establish an HPLC method for determination of the related substances and content of glucosamine hydrochloride products from different manufacturers,and evaluate the quality variation of products of three dosage forms from eight different manufacturers. METHODS The determination method was developed on a Phenomenex Luna NH₂ column(4.6 mm??250 mm,5 ??m) , with phosphate buffer (7.0 g dipotassium hydrogen phosphate dissolved in a suitable amount of water, diluted with 0.5 mL ammonia, add water to 2 000 mL, adjusted to pH 7.5 with phosphoric acid)-acetonitrile (25:75) as mobile phase at a flow rate of 1.5 mL??min^-1. The column temperature was maintained at 30 ?? and detection wavelength was set at 195 nm. RESULTS The system suitability test met the requirements, and the resolution between the peaks of glucosamine hydrochloride and the impurities were greater than 1.5. Good linearity was shown for glucosamine hydrochloride in the concentration range of 0.156 64-15.664 mg??mL^-1 (r=0.999 9). The average recovery rate was 101.14%, with RSD of 1.20% (n=9).CONCLUSION The established method can be applied in the simultaneous determination of the related substances and content of glucosamine hydrochloride products and provide reference for the quality control.     

盐酸消旋山莨菪碱注射液处方的优化研究

目的 优化盐酸消旋山莨菪碱注射液工艺处方,提高产品稳定性。方法 盐酸消旋山莨菪碱注射液工艺处方改为预先配制盐酸溶液,再将消旋山莨菪碱缓缓加入盐酸溶液中,成盐时pH值控制在5.0～5.2。结果 工艺处方更改后,可降低产品的有关物质,提高稳定性。结论 经处方优化后,盐酸消旋山莨菪碱注射液可在室温条件下稳定储存。     

硫酸吗啡原料药中有关物质检查方法研究

目的 通过对硫酸吗啡原料药的有关物质进行分析,考察现行标准的完善性,探讨存在的问题,为提高产品质量标准提供参考。方法 采用HPLC,选用Symmetry C₁₈(4.6 mm×150 mm,5 μm)色谱柱,以1.01 g·L^-1庚烷磺酸钠溶液(用50%磷酸调节pH值至2.6)和甲醇为流动相进行梯度洗脱;检测波长为230 nm,流速为1.5 mL·min^-1,柱温35 ℃。结果 国内硫酸吗啡原料药中检出的主要杂质有可待因(杂质A)、伪吗啡(杂质B)、10-羟基吗啡(杂质D)、吗啡酮(杂质E)和吗啡氮氧化物(杂质F),溶液稳定性显示其中伪吗啡含量增加明显,表明样品需临用新配。结论 建立方法的专属性、线性等均良好,能用于硫酸吗啡原料药中有关物质的检测。现行标准中缺少有关物质检查项,建议增加。     

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??OBJECTIVE To develop a suitable HPLC method combined with component preparation to analyze the related substances and effective contents in bacitracin.METHODS The separation was performed on Agilent HPLC system with a Diamonsil Plus C₁₈ column (4.6 mm??250 mm, 5 ??m) using 50 mmol??L^-1 ammonium formate (pH adjusted to 4.0 with formic acid) as mobile phase A and acetonitrile as mobile phase B at a flow rate of 1 mL??min^-1 under gradient elution. The detection wavelength was set at 254 nm. The HPLC method was carried out by adjusting the pH of ammonium formate solution, the ratio of mobile phase and the solvent. Furthermore, the specificity, linearity, precision, repeatability, stability and durability were studied. The known components like bacitracin A, B1/B2/B3, C1/C2/C3 and F were collected by preparative HPLC according to the HPLC method for bacitracin in USP 40. They were positioned in ammonium formate-acetonitrile HPLC system.RESULTS The established HPLC method was verified to be suitable for analyzing the related substances and effective contents in bacitracin. Baseline separation between the known components and adjacent impurities was achieved, especially the B1/B2. The elution positions of the known component were clearly defined. The contents of the known components in different batches of bacitracin were compared. More detailed sample information was provided in this research.CONCLUSION The HPLC method can simultaneously analyze the related substances and effective contents in bacitracin, and is suitable for the quality control of the product.     

3种注射用盐酸表柔比星溶液的稳定性考察

 目的 考察3种盐酸表柔比星制剂（一种水针剂,两种粉针剂）配制成临床常用溶液后的稳定性。方法 采用0.9%生理盐水,将3种盐酸表柔比星制剂配制成0.4 mg·mL^-1的溶液,分别放置在不同温度,不同避光条件下,定时取样,考察各受试溶液的稳定性,包括样品外观,pH值,样品含量等。结果 3种制剂配制成溶液后在2~8 ℃条件下避光保存40 d,平均含量保留在93.76%以上。室温避光及不避光条件下,仅水针剂配制成溶液后平均含量保持在92.57%以上,另外两种粉针剂在配制成溶液后放置2~7 d,平均含量保留即下降为90%以下。结论 3种盐酸表柔比星制剂配制成溶液后在2~8 ℃条件下保存40 d以及在室温条件下放置1 d均保持稳定,水针剂在室温条件下长期保存（40 d）的稳定性明显优于两种粉针剂。     

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??OBJECTIVE To rapidly identify the related substances in doxycycline hyclate tablets and investigate the possible degradation pathways of doxycycline hyclate solution by 2D-LC-IT-TOF/MS. METHODS Firstly,the chromatography was carried out using the 1stD InertSustain^TM C₁₈(4.6 mm??150 mm,5 ??m) column and a mobile phase containing a mixture of buffer solution(0.25 mol??L^-1 ammonium acetate solution-0.1 mol??L^-1 ethyldiaminetetraacetic acid disodium: triethyiamine=100??10??1)-acetonitrile(85??15). Solution pH was adjusted to 8.8 with glacial acetic acid. Then a InertSustain^TM C₁₈(2.1 mm??50 mm,2 ??m) column was used with 0.1% formic acid-water as mobile A and 0.1% formic acid-acetonitrile as mobile B in a gradient elution mode in 2ndD. Electrospray ionization (ESI) source was tested in both positive and negative ion modes. Nebulized gas flow was 1.5 L?? min^-1. Dry gas flow was 10 L?? min^-1. The desolvation tube temperature was kept at 200 ??. Related substances were characterized according to multi-level MS behaviors. The 2D-LC-IT-TOF/MS method was employed to identify the structures of impurities in forced degradation solutions and illuminate the degradation pathways of doxycycline hyclate solution. RESULTS A total of eight related substances were detected in doxycycline hyclate tablets. Four of them had a content of more than 0.1%, and their structures were identified to be 4-epidoxycycline, metacycline, ??-epidoxycycline and 2-acetyl-2-decarbamoyldoxycycline. The solution of doxycycline hyclate easily degraded under alkaline condition and generated an open loop compound taken off the keto group. The solution was sensitive to heat, and generated 4-epidoxycycline with a little amount of 4-epi-6-epidoxycycline; but the solution was stable under illumination and acidic condition. CONCLUSION The established method is suitable for rapid identification of impurities in doxycycline hyclate, which can be applied as a useful analytical tool for quality control and drug process optimization of doxycycline hyclate.     

梯度洗脱高效液相色谱法检测他克莫司有关物质

 目的建立他克莫司有关物质检测的方法,并观察样品在不同溶剂中可能存在的异构体的转化情况,同时液-质联用技术进一步确证有关物质。方法以辛烷基硅烷键合硅胶为填充剂,以0.02mol·L^-1磷酸二氢钾(pH3.5)与乙腈为流动相梯度洗脱;检测波长为210nm,柱温60℃;利用液-质联用技术确证可能存在的杂质。结果样品在质子性的溶剂中确实存在异构体的转化且该转化能达到平衡,但在乙腈溶剂中基本无转化,该溶剂可作为他克莫司有关物质的测定溶剂,样品中的主要杂质为发酵副产物。结论本法简便、准确,重复性好,能有效地检测样品中的有关物质。     

注射用维生素C的质量研究

目的:进行注射用维生素C的质量研究,为临床用药提供参考。方法:采用高效液相色谱法测定注射用维生素C的有关物质,并对此方法进行验证。结果:有关物质的HPLC测定方法分离度良好,辅料及降解物对测定没有影响。结论:该质量控制方法可靠,本公司和国内首研产品质量指标无显著差异。