HPLC法检查苯甲酸阿格列汀原料药的有关物质

目的:建立检查苯甲酸阿格列汀原料药中有关物质的方法。方法:采用高效液相色谱梯度洗脱法。色谱柱为C18,流动相A为0.2%磷酸溶液(pH 3.0),流动相B为乙腈,以1.0 ml/min流速进行梯度洗脱,检测波长为225 nm,进样量为20μl。采用不加校正因子主成分自身对照法检查特定杂质F-1的量。结果:苯甲酸阿格列汀与F-1及其他未知杂质均分离良好,前二者检查质量浓度线性范围分别为0.187 2⁰.748 8、0.184 50.748 8、0.184 5⁰.738 0μg/ml(r=0.999 7、0.999 9);F-1的检测限和定量限分别为2.5、7.5 ng,平均回收率为100.9%(RSD=1.10%,n=3);3批样品中F-1量均≤0.06%。结论:建立的方法灵敏快速、结果准确可靠,可作为苯甲酸阿格列汀原料药的有关物质检查方法。     

An HPLC method for the determination of atorvastatin and its impurities in bulk drug and tablets

A simple high-performance liquid chromatographic (HPLC) method was developed for the analysis of atorvastatin (AT) and its impurities in bulk drug and tablets. This method has shown good resolution for AT, desfluoro-atorvastatin (DFAT), diastereomer-atorvastatin (DSAT), unknown impurities and formulation excipients of tablets. A gradient reverse-phase HPLC assay was used with UV detection. Some solvent systems prepared using methanol or acetonitrile and water or buffer systems with different pH values were tested. Capacity factors of related substances were calculated at all tested systems. Best resolution has been determined using a Luna C₁₈ column with acetonitrile–ammonium acetate buffer pH 4-tetrahydrofuran (THF) as mobile phase. Samples were eluted gradiently with the mobile phase at flowrate 1.0 ml min⁻¹ and detected at 248 nm. The proposed method was applied to the determination of impurities and were found to contain 0.057–0.081, 0.072–0.097, 0.608–0.664% of the DFAT, DSAT and total impurity, respectively.     

A stability-indicating HPLC method for medroxyprogesterone acetate in bulk drug and injection formulation

A stability-indicating HPLC assay method has been developed and validated for medroxyprogesterone acetate (MPA) in bulk drug and injectable suspension. An isocratic RP-HPLC was achieved on a Hichrom C₁₈ column (150 mm × 4.6 mm i.d., 5 μm) utilizing a mobile phase of methanol 0.020 M acetate buffer pH 5 (65:35, v/v) and a photodiode array detector at 245 nm. The stress testing of MPA was carried out under acidic and alkaline hydrolysis, and oxidation conditions. MPA was well resolved from its degradation products, a main related substance (megestrol acetate) and two preservatives (methyl paraben and propyl paraben) with the resolution ≥2. The proposed method was validated for selectivity, linearity, accuracy, precision and solution stability. The method was found to be suitable for the quality control of MPA in bulk drug and injections as well as the stability-indicating studies.     

HPLC法测定苯甲酸利扎曲普坦片中主药的含量

目的:建立以高效液相色谱法测定苯甲酸利扎曲普坦片中主药含量的方法。方法:色谱柱为C18,流动相为乙腈-水(用醋酸调节pH至3·4,25:75),检测波长为227nm,进样量为20μL,流速为1mL·min-1。结果:苯甲酸利扎曲普坦检测浓度的线性范围为0·001～0·200mg·mL-1(r=0·9999);平均回收率为100·78%(RSD=0·15%)。结论:本方法灵敏、可靠、选择性高,适用于该制剂的质量控制。     

高效液相色谱法测定苯甲酸利扎曲普坦片含量及含量均匀度

目的采用高效液相色谱法测定苯甲酸利扎曲普坦片含量及含量均匀度.方法色谱条件为Prodigy ODS C18硅烷键合硅胶填充柱(150 mm×4.6 mm,5 μm);流动相为乙腈-0.025%磷酸二氢钾-三乙胺(36∶264∶1),10%磷酸调pH 5.0;检测波长为225 nm;进样量为20 μL;流速为1.0 mL*min-1.结果在进样量为0.101～1.01 μg,样品浓度和峰面积成良好线性关系,r=0.999 9,平均回收率为101.20%,RSD为2.2%. 结论方法灵敏可靠,选择性高.     

HPLC法测定兰索拉唑肠溶片的血药浓度

目的建立HPLC法测定兰索拉唑肠溶片的血药浓度。方法采用高效液相色谱法,色谱柱:Hypersil ODS(250 mm×4.6 mm,5μm),柱温:40℃,流动相为水∶乙腈∶正辛胺(620∶380∶1),流速:1.2 ml.min-1,检测波长:285 nm。结果兰索拉唑在0.05～2.00 mg.L-1范围内线性关系良好(r=0.999 8),平均回收率为99.48%,RSD=4.50%。结论该方法灵敏、准确、稳定,适用于兰索拉唑的血药浓度检测。     

珍黄片所用药材的鉴别及黄芩苷的测定

目的鉴别珍黄片所用药材并测定其中的黄芩苷。方法采用TLC法和HPLC法。结果鉴定了珍黄片中珍珠、黄芩提取物、牛黄、猪胆汁、三七、薄荷油、冰片共七味药材,黄芩苷的回归方程为:W=7.32×10-8A 3.57×10-4(r=0.9998,n=6),黄芩苷0.011~0.570μg与峰面积呈良好的线性关系。结论所建方法简便、准确,能有效地控制珍黄片的质量。     

Gradient high performance liquid chromatography method for simultaneous determination of ilaprazole and its related impurities in commercial tablets

A methodology (HPLC) proposed in this paper for simultaneously quantitative determination of ilaprazole and its related impurities in commercial tablets was developed and validated. The chromatographic separation was carried out by gradient elution using an Agilent C₈ column (4.6 mm × 250 mm, 5 μm) which was maintained at 25 °C. The mobile phase composed of solvent A (methanol) and solvent B (solution consisting 0.02 mmol/l monopotassium phosphate and 0.025 mmol/l sodium hydroxide) was at a flow rate of 1.0 ml/min. The samples were detected and quantified at 237 nm using an ultraviolet absorbance detector. Calibration curves of all analytes from 0.5 to 3.5 μg/ml were good linearity (r ≥ 0.9990) and recovery was greater than 99.5% for each analyte. The lower limit of detection (LLOD) and quantification (LOQ) of this analytical method were 10 ng/ml and 25 ng/ml for all impurities, respectively. The stress studies indicated that the degradation products could not interfere with the detection of ilaprazole and its related impurities and the assay can thus be considered stability-indicating. The method precisions were in the range of 0.41–1.21 while the instrument precisions were in the range of 0.38–0.95 in terms of peak area RSD% for all impurities, respectively. This method is considered stability-indicating and is applicable for accurate and simultaneous measuring of the ilaprazole and its related impurities in commercial enteric-coated tablets.     

HPLC analysis,semi-preparative HPLC preparation and identification of three impurities in salidroside bulk drug

Salidroside is a bioactive compound mainly distributed in Rhodiola L. (Crassulaceae). It has been widely used in Chinese traditional medicine. In this paper, three impurities were found during the analysis of salidroside bulk drug. The enrichment of impurities was carried out by ODS column chromatography, using methanol–water (13:87, v/v) as eluent and the purification of impurities was achieved by semi-preparative HPLC, using methanol–water (11:89, v/v) as mobile phase, respectively. Three impurities were characterized as 4-(2-hydroxylethyl)-phenol-1-O-β-d-glucopyranoside, 4-hydroxyphenacyl-d-glucopyranoside and p-acetylphenyl-O-β-d-glucopyranoside by a variety of spectral data (IR, UV, MS, ¹H NMR, ¹³C NMR, DEPT and 2D NMR). The simultaneous quantitative determination of salidroside and its impurities (Imp. 1, 2 and 3) was performed by reverse-phase HPLC method with UV detection. Specificity, linearity, sensitivity, precision and accuracy were evaluated.     

瑞香素缓释片中瑞香素含量测定方法的建立与验证

目的建立一种测定瑞香素缓释片中瑞香素含量的高效液相色谱法（HPLC）并对其进行验证。方法色谱柱为Agela Venusil C18（4.6 mm×250 mm,5μm）,流动相为甲醇-0.05%磷酸溶液（45∶55）,流速1.0 ml/min,柱温30℃,检测波长323 nm,进样量10μl。结果瑞香素在5～45μg/ml范围内具有良好的线性关系,R2=0.9999,平均回收率为101.17%,RSD为0.3%。结论该法准确可靠,操作简便,可用于瑞香素缓释片的含量测定。     

Development and application of a validated HPLC method for the determination of gabapentin and its major degradation impurity in drug products

A simple isocratic reversed-phase HPLC method for the determination of gabapentin and its major degradation impurity, 3,3-pentamethylene-4-butyrolactam, was developed and validated for use in the analysis of pharmaceutical tablets and capsules. Separation was achieved on a Brownlee Spheri-5 Cyano column using an acetonitrile–10 mM KH₂PO₄/10 mM K₂HPO₄ (pH 6.2) (8:92, v/v) mobile phase. The compounds were eluted isocratically at a flow rate of 1 mL/min. Both compounds were analyzed with UV detection at 210 nm. The method was validated according to USP Category I requirements for gabapentin and USP Category II for 3,3-pentamethylene-4-butyrolactam. The validation characteristics included accuracy, precision, linearity, range, specificity, limit of quantitation and robustness. Validation acceptance criteria were met in all cases. This method was used successfully for the quality assessment of four gabapentin drug products.     

高效液相色谱法测定爱普列特片的含量和溶出度

目的:建立测定爱普列特片的含量和溶出度的高效液相色谱法。方法:色谱柱为北京迪马 Diamonsil~(TM)C_(18)柱(250 mm×4.6 mm,5μm),流动相为甲醇-异丙醇-水(82:3:15),检测波长为266 nm。按中国药典转篮法,采用天津大学无线电厂ZRS-8G 智能溶出试验仪,以0.001 mol·L~(-1)氢氧化钠溶液为溶出介质测定溶出度。结果:在0.5～20 mg·L~(-1)浓度范围,爱普列特的峰面积与浓度呈良好线性关系(r=0.9998),加样回收率为98.3%,相对标准偏差为1.2%(n=5)。5 min 溶出为42%～51%,10 min 溶出超过65%,3批片剂的50%溶出时间 T_(50)为3.4～6.1 min。结论:方法简便可靠,能够满足爱普列特片含量和溶出度测定的要求。     

高效液相色谱法测定马来酸氨氯地平片的含量

目的 建立高效液相色谱法测定马来酸氨氯地平片的含量。方法 采用Kromasil C18柱(5 μm,4.6 mm×250 mm);以甲醇-0.05mol?L-1乙酸铵溶液(70:30)为流动相[1];检测波长365 nm[2、3];流速1.0 ml?min-1。结果 马来酸氨氯地平在22.4~336.0 μg?mL-1的线性范围内呈良好的线性,r=0.9999(n=6),平均回收率为99.4%,RSD=0.29%(n=9)。结论 该方法简便、快速、准确、专属性好,适于马来酸氨氯地平片含量控制。     

HPLC法测定六昧安消片中大黄素和大黄酚的含量

目的:建立六味安消片中大黄素和大黄酚的含量测定方法。方法:用 HPLC 方法对制剂中大黄中所含的大黄素和大黄酚进行含量测定研究。采用 Inertsil ODS-3(5μm,250mm×4.6mm)柱,以甲醇-0.1%磷酸水溶液(85:15)为流动相,检测波长为254nm。结果:大黄素在0.0144～0.072μg范围内呈线性关系(r=0.9997,n=5),平均回收率为97.24%;大黄酚在0.035～0.175μg范围内呈线性关系(r=0.9999,n=5),平均回收率为99.35%。结论:本方法操作简便、可靠,重现性好,专属性强,可作为六味安消片的内在质量控制方法。     

醋酸地塞米松片及其有关物质分析

目的:进一步考察醋酸地塞米松片剂的质量,检测有关物质,防止掺假。方法:采用薄层色谱法和高效液相色谱法,薄层色谱条件,硅胶 G_(F254)板10×20 cm,展开剂二氯甲烷-甲醇(18:2),在254nm 波长下检视。高效液相色谱法 C_(18)反相柱,流动相:甲醇-水(70:30),检测波长在240nm 或254nm,流速0.8mL·min~(-1),r=0.9999。结果:在 TLC 条件下,可检出主成分及有关物质,HPLC 可准确定量主成分,同时检测有关物质。结论:采用薄层色谱法和高效液相色谱法,可测定醋酸地塞米松片及其有关物质,该方法准确灵敏,也可用于药物快速检验。     

HPLC法测定富马酸氯马斯汀及富马酸氯马斯汀片的有关物质

目的:采用高效液相色谱法测定富马酸氯马斯汀及片剂中的有关物质和降解产物。方法:采用ODS-3 C18色谱柱(250mm×4.6 mm,5μm);柱温为35℃;流动相为乙腈-辛烷磺酸钠溶液(50∶50);流速为1.0 mL.min-1;检测波长为210 nm;进样量为10μL。结果:各降解产物、辅料均可与富马酸氯马斯汀主峰良好分离,方法的精密度和重复性良好(RSD<0.3%)。结论:经方法学验证,该法灵敏、准确,适用于富马酸氯马斯汀及片剂中有关物质的测定。