附子理中丸(浓缩丸)质量标准的建立

目的:建立附子理中丸（浓缩丸）质量控制方法。方法:采用薄层色谱法对方中干姜、甘草进行定性鉴别;采用高效液相色谱法测定样品中甘草苷含量。色谱柱为Agilent Zorbax-SB C₁₈（250 mm×4.6 mm,5μm）,流动相:乙腈-0.5%醋酸溶液（20:80）,柱温:35℃,流速:0.8 ml·min^-1,检测波长:276 nm。结果:薄层定性鉴别的斑点清晰,分离效果良好;甘草苷对照品在0.016～0.477μg范围内线性关系良好（r=0.999 9）,平均回收率为98.11%,RSD为1.12%（n=9）。结论:本法简便、可靠、准确,可用于该制剂的质量控制。     

当归调经颗粒质量标准研究

目的建立当归调经颗粒的质量标准。方法采用薄层色谱法对处方中的当归、甘草、白芍等药材进行鉴别;采用高效液相色谱法测定芍药苷的含量：色谱柱为Hypersil ODS C18柱（250mm×4.60mm,5μm）;流动相为甲醇-水（32∶68）,流速1.0mL.min-1;检测波长为233nm;柱温30℃,进样量为10μL。结果当归、甘草、白芍薄层色谱斑点清晰、分离度好。HPLC法测定芍药苷含量,芍药苷在0.0912~2.622μg范围内线性关系良好,平均回收率为100.26%,RSD为2.86%。结论所建立的质量标准简便可行、重复性好,可用于当归调经颗粒的质量控制。     

双芩清解颗粒的质量标准研究

目的：建立双芩清解颗粒的质量标准。方法：采用薄层色谱法对方中的黄芩、知母、板蓝根3味药材进行鉴别;采用高效液相色谱法测定黄芩苷的含量：色谱柱为Syncronis C18（250 mm ×4.6 mm,5μm）;流动相为甲醇-0.1%甲酸（44∶56）;流速1.0 ml·min^-1;检测波长为278 nm;柱温35℃;进样量为10μl。结果：黄芩、知母、板蓝根薄层色谱斑点清晰、分离度好、专属性强。黄芩苷在0.062~2.184μg（r=0.9999）范围内线性关系良好,平均加样回收率为101.34%,RSD为1.10%（n=5）。结论：所建立的质量标准简便可行、重复性好,可用于双芩清解颗粒的质量控制。     

反相高效液相色谱法测定黄芩苷固体分散体中黄芩苷的含量

目的建立反相高效液相色谱法测定黄芩苷固体分散体中黄芩苷含量的测定方法。方法采用DiamonsilC18色谱柱（250mm×4.6mm,5μm）,以甲醇-0.1%磷酸溶液（55∶45）为流动相,柱温为30℃,流速为1.0ml/min,检测波长280nm,进样量为10μl。结果黄芩苷浓度在29.0～174.0μg/ml的范围内与峰面积呈良好的线性关系,线性方程为A=21.809C-17.243（r=1.0000,n=7）;黄芩苷的平均回收率为100.9%,RSD值为1.18%。该方法的精密度、重复性良好,RSD值均小于2.00%。结论该方法简便、快捷、准确度高,能有效控制黄芩苷固体分散体胶囊中黄芩苷的质量。     

高效液相色谱法测定咽炎茶中黄芩苷含量

目的建立咽炎茶中黄芩苷含量测定的高效液相色谱法。方法色谱柱为ODS柱（4.6mm×250mm,5μm）,流动相为甲醇-水-磷酸（30∶70∶1）,流速为1.0mL/min,检测波长为280nm,进样10μL。结果黄芩苷在0.1988~1.1928μg范围内线性关系良好,r=0.9997,平均回收率为97.4%,RSD=1.1%。结论本方法稳定可行,结果准确可靠,可作为咽炎茶质量标准中黄芩苷的含量测定方法。     

调经活血胶囊质量标准研究

目的 提高完善调经活血胶囊质量标准.方法 采用薄层色谱法对丹参、熟地黄进行鉴别;采用高效液相色谱法测定赤芍中芍药苷含量,色谱柱为Agilent Zorbax-SB C18（250mm×4.6mm,5μm）,流动相为甲醇-水（25：75）,柱温：35℃,流速：0.8mL·min-1,检测波长：230nm.结果 薄层色谱斑点清晰,分离效果良好;芍药苷对照品在0.01201～2.156μg范围内线性关系良好（r=0.9996）,平均回收率为96.61%,RSD为1.21% （n=9）.结论 本法简便、可靠、准确,可用于该制剂的质量控制.     

阿归养血颗粒质量标准研究

目的 提高并完善阿归养血颗粒的质量标准。方法 采用薄层色谱（TLC）法对白芍、黄芪、甘草进行鉴别,采用高效液相色谱（HPLC）法对当归和川芎进行鉴别;同时采用HPLC法测定芍药苷的含量,色谱柱为Agilent TC-C18柱（250 mm×4.6 mm,5μm）,流动相为乙腈-水（10∶90）,流速为1.0 mL/min,检测波长为230 nm。结果 TLC法色谱斑点清晰,专属性强,重复性良好。芍药苷对照品进样量在0.048 56～0.971 2μg（r=0.999 9）范围内与峰面积呈良好线性关系,平均回收率为99.47%,RSD为1.23%（n=6）。结论 该方法简便、可靠、准确,可用于该制剂的质量控制。     

高效液相色谱法测定舒肝颗粒中黄芩苷和阿魏酸的含量

目的：建立舒肝颗粒的质量标准。方法：采用薄层色谱法（TLC）对其中柴胡、当归进行鉴别;建立高效液相色谱（HPLC）法测定其中黄芩苷和阿魏酸的含量,色谱柱：HYPERSIC ODS C₁₈柱（4.6 mm×200 mm,5 μm）;流动相：乙腈-0.1%磷酸溶液（22∶78）;流速：1.0 mL·min^-1;检测波长：280 nm;柱温：30℃。结果：TLC鉴别柴胡对照药材、当归对照药材均具有良好的分离效果,阴性对照无干扰;高效液相色谱（HPLC）法黄芩苷在12.64~126.40 μg·mL^-1范围内线性关系良好,r=0.999 7,平均回收率为97.7%（RSD=1.02%）;阿魏酸在9.46~94.60 μg·mL^-1范围内线性关系良好,r=0.999 9,平均回收率为97.5%（RSD=1.22%）。结论：所建立的薄层鉴别方法专属性强,含量测定方法简便,准确,可用于舒肝颗粒的质量控制。     

清热解毒合剂的质量标准研究

目的:建立清热解毒合剂的质量标准。方法:采用薄层色谱法对清热解毒合剂中平贝母、甘草、紫苑、麦冬进行鉴别,采用高效液相色谱法测定本制剂主成分黄芩中黄芩苷含量。结果:薄层色谱斑点清晰,分离良好,阴性对照液无干扰。黄芩苷进样量在0.157~0.785μg范围内线性关系良好,平均加样回收率为97.5%(n=5),RSD为1.6%。结论:本方法可作为清热解毒合剂的质量控制方法。     

高效液相色谱法测定炎可宁片中黄芩苷的含量

目的应用HPLC法测定炎可宁片中黄芩苷的含量。方法液相色谱法。色谱柱为Kromasil C18柱（4.6mm×250mm,5μm）;流动相：甲醇-冰醋酸-水（50∶1∶50）;流速1.0mL.min-1;柱温：30℃;检测波长316nm。结果黄芩苷在0.4436~5.545mg.L-1范围内呈线性关系（r=1.0000,n=6）,平均加样回收率为100.09%,RSD为1.41%（n=9）。结论该方法简便快速,结果准确,可用于炎可宁片中黄芩苷含量的测定。     

高效液相色谱-四极杆飞行时间质谱法鉴定头孢他啶原料药的有关物质

目的： 采用高效液相色谱-四极杆飞行时间质谱法（HPLC-Q-TOF-MS）对头孢他啶原料药中有关物质进行分离和结构鉴定。方法： 色谱条件：采用Agilent ZORBAX RX-C₁₈色谱柱（150 mm×2.1 mm,5 μm）,以乙腈-0.1%甲酸水为流动相,流速0.2 mL·min^-1,紫外检测波长254 nm;质谱条件：采用正离子扫描（ESI⁺）方式,在m/z 100~1 200范围内进行质谱扫描;结合头孢他啶与已知结构有关物质的多级质谱裂解规律,鉴定所有有关物质的结构。结果： 获得了头孢他啶原料药中13个有关物质的精确质量数和结构式,除杂质1和5外,其余11种均为尚未报道的未知杂质。结论： 本高分辨液质联用方法能同时有效地鉴定头孢他啶原料药中的小分子杂质和聚合物杂质,为其生产工艺和质量控制提供重要的检测手段和参考依据。     

LC determination of rosiglitazone in bulk and pharmaceutical formulation

An isocratic reversed phase liquid chromatographic (RP-LC) method has been developed and subsequently validated for the determination of rosiglitazone and its related impurities. Separation was achieved with a Symmetry C18 column and sodium phosphate buffer (pH adjusted to 6.2):acetonitrile (50:50, v/v) as eluent, at a flow rate of 1.0 ml/min. UV detection was performed at 245 nm. The method is simple, rapid, selective and stability indicating. Indole was used as internal standard for the purpose of quantification of rosiglitazone. The described method is linear over a range of 0.45-10 microg/ml for related impurities and 180-910 microg/ml for assay of rosiglitazone. The method precision for the determination of assay and related compounds was below 1.0 and 3.6% RSD, respectively. The mean recoveries of impurities were found to be in the range of 95-102%. The percentage recoveries of Active Pharmaceutical Ingredient (API) from dosage forms ranged from 99.02 to 101.30. The method is useful in the quality control of bulk manufacturing and also in pharmaceutical formulations.     

Determination of isepamicin sulfate and related compounds by high performance liquid chromatography using evaporative light scattering detection

A simple reversed phase high performance liquid chromatographic method was developed for the analysis of isepamicin sulfate. The use of evaporative light scattering detection eliminates the need for sample derivatization. Separation of the isepamicin aminoglycoside from structurally similar related compounds was achieved using two Waters X-Terra RP18 columns connected in tandem at 10 degrees C. The assay of isepamicin sulfate and the estimation of its impurities was accomplished using external standard calibration curves at two sample concentrations: 1.6 mg ml(-1) for the analysis of isepamicin sulfate and 8.0 mg ml(-1) for the estimation of lower level impurities. The limit of detection was 0.1%. The specificity, assay linearity, low level assay linearity and assay repeatability were also investigated.     

Determination of 1-benzo[b]thien-2-ylethanone and related impurities by high performance liquid chromatography

1-Benzo[b]thien-2-ylethanone (2-acetylbenzothiophene, 2-ABT) and related impurities were determined using a reverse-phase high performance liquid chromatography system and UV detection at 254 nm. Separation was achieved isocratically on a 4.6 mm × 25 cm, 5 μm Zorbax Rx-C8 column using an eluent which is 0.2% perchloric acid/THF in a ratio of 60:40 (v/v). The chromatographic system resolved 2-ABT and known impurities in less than 45 min with near baseline resolution. Known impurities were quantitated versus 2-ABT with corrections made for differences in detector response at the specified wavelength. Linearity for 2-ABT was demonstrated with a correlation coefficient > 0.9999. Assay precision (RSD values) for impurities at 0.5% ranged from ±1.8% to ± 14%, while precision (RSD values) for the 2-ABT determination ranged from ±0.81% to ±1.1%. A variety of different chromatographic columns and conditions are discussed for the application.     

A validated reversed phase HPLC method for the determination of process-related impurities in almotriptan malate API

An isocratic reversed phase liquid chromatographic (RP-LC) method has been developed and subsequently validated for the determination of almotriptan malate and its process-related impurities. Separation was achieved with a Phenomenex, Gemini, C-18 column and sodium phosphate buffer (pH adjusted to 7.6): acetonitrile (80:20, v/v) as eluent, at a flow rate of 1.5 mL/min. UV detection was performed at 227 nm. The method is simple, rapid, selective, accurate and stability indicating. The described method is linear over a range of LOQ, 1.5 ug/mL (150% of the specification limit) for all the process-related impurities. The method precision for the determination of related compounds was below 1.0% R.S.D. The accuracy of the method demonstrated at 4 levels in the range of 25-150% of the specification limit and the recovery of impurities were found to be in the range of 96-102%. The method is useful in the quality control of bulk manufacturing.     

Combined assay, identification, and foreign related steroids test for methandrostenolone by high-speed liquid chromatography.

A high-speed liquid chromatographic system is described, which can be used for the simultaneous identification of the anabolic steroid methandrostenolone and its impurities and the quantitation of each of these compounds. Separation is effected by adsorption chromatography on a slurry-packed microparticulate silica gel column.     

青霉素单克隆抗体致敏羊红血球的反向间接血凝试验检测氨苄青霉素中致敏性杂质

采用青霉素单克隆抗体致敏羊红血球的反向间接血凝试验,可以快速、简单、高灵敏度及专属性强的检测氨苄青霉素中致敏性杂质,其结果与皮肤被动过敏试验相平行,不同批号氨苄青霉素样品含杂质量有差别,氨苄青霉素中致敏性高分子杂质含量比青霉素高,可能与其过敏反应率较高有关.     

液质联用快速确定尼群地平原料药中的杂质

目的:利用液质联用技术对尼群地平原料药中的2个杂质进行在线的质谱分析。方法:采用C18(250 mm×4.6 mm,5μm)色谱柱,流动相为甲醇-水(70︰30),流速为1.0 mL.min-1;Agilent 6320质谱仪,离子源为ESI,质量分析器为离子阱,检测模式为正离子。结果:直接推断出了2个杂质可能的化学结构。结论:检测结果对于尼群地平原料药的杂质分析、质量控制和合成工艺的改进具有重要作用。     

LC and LC–MS/MS study of forced decomposition behavior of anastrozole and establishment of validated stability-indicating analytical method for impurities estimation in low dose anastrozole tablets

Anastrozole tablets were subjected to different ICH prescribed stress conditions of thermal, hydrolysis, humidity, photolysis and oxidation stress. The drug was found to be stable for all the stressed conditions except for oxidation. Separation of anastrozole from its potential impurities, degradation products and five anastrozole related compounds as main impurities were achieved on Inertsil ODS-3V, 250 mm × 4.6 mm i.d, 5 μm analytical column using reversed phase high performance liquid chromatography (RP-HPLC). The elution of impurities employed time dependent gradient programmed mobile phase consisting of water as mobile phase-A and acetonitrile as mobile phase-B at column flow rates of 1 ml/min and at 215 nm UV detection. The same method was also extended to LC–MS/MS studies which were carried out to identify the degradation product. The method developed was established to have sufficient intermediate precision as similar separation was achieved on another instrument handled by a different operator. The LOQ for anastrozole related compound-A (RC-A), related compound-B (RC-B), related compound-C (RC-C), related compound-D (RC-D), related compound-E (RC-E) and anastrozole were 0.05, 0.03, 0.03, 0.06, 0.06 and 0.06 μg ml⁻¹ respectively. The linearity of the proposed method for all the above related compounds was investigated in the range of LOQ to 0.600 μg ml⁻¹ respectively. The specificity was established through peak purity testing using a photo-diode array detector. Method was validated according to ICH guidelines and statistical analysis of the data proved to be suitable for stability testing at quality control.     

A new validated liquid chromatographic method for the determination of loratadine and its impurities

An improved gradient, reversed-phase liquid chromatographic (RP-LC) method was developed and subsequently validated for the determination of Loratadine and its impurities/degradation products in pharmaceutical drug substance. Separation was achieved with Inertsil ODS-3V, 250 × 4.6 mm, 5μ column with gradient elution at a flow rate of 1.0 mL min(-1). UV detection was performed at 220 nm. The described method is linear over a range of LOQ (0.044, 0.088, 0.084, and 0.072 μg mL(-1) for impurity-B, impurity-C, impurity-D, and impurity-E respectively) to 1.2 μg mL(-1) (0.6 μg mL(-1) of the specification limit) for all the impurities and degradation products. The recovery of impurities were found to be in the range of 85-115 %. The method is simple, selective, and accurate for the quantification of impurities and degradation products of Loratadine in its bulk drug samples.