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排序方式: 共有171条查询结果,搜索用时 15 毫秒
1.
目的 建立醋酸亮丙瑞林注射液中亮丙瑞林及杂质的测定方法。方法 采用高效液相色谱法。色谱柱 :Kromasil C18-ODS(150mm×4.6mm ,5 μm)不锈钢柱 ;流动相 :水相 (800ml水 +21ml三乙胺 ,磷酸调pH 3.0 ,加水至 1000ml)-有机相 (正丙醇-乙腈 =2∶3)为 84∶16 ;检测波长:220nm ;含量测定采用外标法 ,杂质检查采用自身对照法。结果 在优化的色谱条件下 ,亮丙瑞林及杂质间均能完全分离 ,注射液辅料不干扰测定 ,亮丙瑞林线性范围 9.198~ 82.780 μg·ml-1,检测限 1.93ng(S/N =3) ,含量测定的回收率 98.74%~100.3% ,RSD<1.5%。结论 该法专属性强,操作方便 ,结果准确 ,重现性好。 相似文献
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Lakkireddy Prakash Malipeddi Himaja Belly Ramakrishna Yadav Arumalla Maheshwara Reddy 《Scientia pharmaceutica》2015,83(3):453-463
Cost-effective isolation methods were developed on preparative HPLC, flash LC, and simulated moving bed (SMB) to prepare the process impurity, 3-(aminomethyl)-5-methylhex-4-enoic acid (4-ene impurity), of pregabalin. By a thorough experimental study on the different isolation techniques available, it was concluded that SMB was the most cost-effective. Hence, it was a continuous chromatography that utilized the advantage of SMB so that a high quantity of the impurity was generated in a short period of time. SMB was equipped with eight reversed-phased columns and was used to separate the process impurity of pregabalin. The effects of flow rate in zone 2 (Q2) and 3 (Q3), as well as switching time, on the operating performance parameters like purity, productivity, and desorbent consumption were studied. Operating conditions leading to more than 90% purity in the raffinate outlet stream were identified, together with those achieving optimal performance. All of these developed methods are novel, cost-effective, and can be applied to the isolation of other process- and stability-related impurities of pregabalin. 相似文献
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目的 建立莫匹罗星软膏有关物质HPLC分析方法。方法 采用Agilent Zorbax C8(250mm×4.6mm, 5μm)色谱柱,柱温:30℃,流动相:以pH5.7乙酸铵溶液-四氢呋喃不同比例线性梯度洗脱,流速:0.8mL/min,检测波长:240nm,进样量:20μL。结果 莫匹罗星及莫匹罗星杂质C、D、E分别在25~100μg/mL浓度范围内线性关系良好;定量限分别为0.016、0.047、0.019及0.020μg;杂质C、D和E的平均回收率分别为103.7%、98.6%和93.9%;重复性RSD均小于1.0%;酸、碱、高温、氧化、光照强制降解试验证明方法的专属性良好。结论 所建立的方法专属性、准确性及耐用性均良好,可用于莫匹罗星软膏有关物质的检测。 相似文献
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目的 建立头孢地尼原料及制剂聚合物杂质的分析方法。方法 分别采用0.1mol/L磷酸盐溶液和氯仿-三乙胺为溶剂,制备头孢地尼降解溶液;采用高效凝胶色谱法(HPSEC, TSK G2000 SWxl)和柱切换-LC/MSn法对头孢地尼降解溶液的弱保留值杂质进行分离和结构鉴定,并评估高效凝胶色谱法分析聚合物杂质的专属性;采用Diamonsil, C18型色谱柱,以0.25%四甲基氢氧化铵溶液(pH5.5)-甲醇-乙腈为流动相进行梯度洗脱,建立头孢地尼聚合物的RP-HPLC分析方法,采用二维色谱法和柱切换-LC/MSn法对其专属性进行分析,并进行方法学验证。结果 在头孢地尼降解物中鉴定出头孢地尼二聚体及其异构体,以及若干小分子杂质;高效凝胶色谱法分离头孢地尼聚合物杂质时,小分子杂质与聚合物杂质共出峰,方法专属性与定量准确性差;RP-HPLC法分析头孢地尼聚合物杂质时,能够检出头孢地尼二聚体及其异构体,头孢地尼三聚体,专属性好。结论 高效凝胶色谱法不能对头孢地尼的聚合物杂质进行有效质控,建立的反相色谱法分析头孢地尼聚合物杂质的专属性良好,可将头孢地尼降解溶液可作为聚合物杂质系统适用性溶液。 相似文献
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目的 建立二维超高效液相色谱质谱联用法研究注射用头孢地嗪钠的杂质谱。方法 一维色谱采用Waters HSS T3 C18(100mm×2.1mm, 1.8μm);以磷酸盐缓冲液(取磷酸二氢钾0.87g,无水磷酸氢二钠0.22g,加水溶解并稀释至1000mL)为流动相A,乙腈为流动项B,梯度洗脱;柱温:35℃;流速:0.4mL/min;检测波长:215nm;进样量:3μL;二维色谱采用Waters BEH C18(50mm×2.1mm, 1.7μm);以0.1%甲酸水溶液为流动相A,0.1%甲酸的乙腈为流动项B,切峰后开始B相3min由2%到95%;柱温:35℃;流速:0.4mL/min;质谱采用Xevo G2-XS QTof MS系统,离子源为ESI源,离子源温度:110℃,毛细管电压:3.0KV,雾化器温度:450℃,雾化器流速:800L/h,扫描范围:m/z 100~2000,测定头孢地嗪主要杂质的一级和二级质谱,进行结构解析。结果 采用UPLC梯度洗脱方法可检出多种头孢地嗪异构体、降解杂质和高分子杂质等,检出杂质的个数和总量均较现行法定标准多。结论 本品的杂质在原料合成、制剂分装及运输储藏过程中均可产生,因此,应对原料和制剂生产过程中的关键技术指标和环境条件加以控制。 相似文献
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Simultaneous detection and quantitation of organic impurities in methamphetamine by ultra‐high‐performance liquid chromatography–tandem mass spectrometry,a complementary technique for methamphetamine profiling
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The analysis of organic impurities plays an important role in the impurity profiling of methamphetamine, which in turn provides valuable information about methamphetamine manufacturing, in particular its synthetic route, chemicals, and precursors used. Ultra‐high‐performance liquid chromatography – tandem mass spectrometry (UHPLC – MS/MS) is ideally suited for this purpose due to its excellent sensitivity, selectivity, and wide linear range in multiple reaction monitoring (MRM) mode. In this study, a dilute‐and‐shoot UHPLC – MS/MS method was developed for the simultaneous identification and quantitation of 23 organic manufacturing impurities in illicit methamphetamine. The developed method was validated in terms of stability, limit of detection (LOD), lower limit of quantification (LLOQ), accuracy, and precision. More than 100 illicitly prepared methamphetamine samples were analyzed. Due to its ability to detect ephedrine/pseudoephedrine and its high sensitivity for critical target markers (eg, chloro‐pseudoephedrine, N‐cyclohexylamphetamine, and compounds B and P), more impurities and precursor/pre‐precursors were identified and quantified versus the current procedure by gas chromatography – mass spectrometry (GC – MS). Consequently, more samples could be classified by their synthetic routes. However, the UHPLC – MS/MS method has difficulty in detecting neutral and untargeted emerging manufacturing impurities and can therefore only serve as a complement to the current method. Despite this deficiency, the quantitative information acquired by the presented UHPLC – MS/MS methodology increased the sample discrimination power, thereby enhancing the capacity of methamphetamine profiling program (MPP) to conduct sample‐sample comparisons. 相似文献
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RP-HPLC法测定酮洛芬凝胶中药物含量 总被引:1,自引:0,他引:1
目的建立酮洛芬凝胶中药物含量测定的方法,并明确光照对含量测定的影响。方法采用Diamonsil ODS柱(4.6 mm×200 mm,5μm);流动相为0.01 mol/L磷酸二氢钾溶液(用磷酸调pH值至3.0)-乙腈(50∶50),流速1.0 mL/min,检测波长为255 nm,柱温为室温。结果在本试验条件下,酮洛芬凝胶中与辅料及有关物质分离度均符合要求,酮洛芬进样量在0.5251.575μg范围内线性关系良好(r=0.999 9,n=5),平均回收率为98.41%,RSD为1.35%(n=3)。经光照,酮洛芬含量明显降低,杂质A明显增加,杂质A为酮洛芬的光照降解产物。结论本方法简单、快捷,可用于酮洛芬凝胶中药物含量的测定。 相似文献
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《Asian Journal of Pharmaceutical Sciences》2015,10(2):152-158
Alogliptin (AGLT), active ingredient of Alogliptin Benzoate (AGLT-BZ), is a new dipeptidyl peptidase-4 (DPP-4) inhibitor for the treatment of type 2 diabetes. This study aimed to build a suitable method to determine the potential related substances in AGLT-BZ bulk drug and tablets. Seven related substances in Alogliptin Benzoate substances were synthetized and identified by 1H-NMR and ESI-MS. In addition, the impurities were detected by a gradient reverse-phase high performance liquid chromatography (RP-HPLC) with UV detection. The chromatographic system consisted of an Angilent Zobax SB-CN column (250 × 4.6 mm; 5 μm). The mobile phase consisted of water/acetonitrile/trifluoroacetic acid 1900:100:1 v/v/v (solution A) and acetonitrile/water/trifluoroacetic acid 1900:100:1 v/v/v (solution B) using a gradient program at a flow rate of 1.0 ml/min with 278 nm detection and an injection volume of 20 μl. Additionally, selectivity, the limit of quantitation (LOQ) and limit of detection (LOD), linearity, accuracy, precision and robustness were determined. Linearity was good over the concentration range 50–1000 ng/ml and the coefficient of determination (R2) were 0.9991–0.9998. RSD% of the determination of precision were <2% (n = 6). The method of RP-HPLC for the determination of impurities in AGLT-BZ was proved to be precise, accurate, robust and reliable. Three batches of self-made bulk drug and three dosages of commercial tablets were detected with this method. 相似文献