Simultaneous determination of artemether and lumefantrine in fixed dose combination tablets by HPLC with UV detection

This paper describes the development and validation of a HPLC-UV method (210 nm) for the simultaneous quantitation of artemether and lumefantrine in fixed dose combination tablets. The method showed to be linear (r(2)>0.99), precise (R.S.D.<2.0%), accurate (recovery of 101.07% for artemether and 101.58% for lumefantrine), specific and robust. Four batches of artemether-lumefantrine tablets were assayed by the validated method. The artemether contents in the tablets varied from 98.61% to 103.35%, while lumefantrine contents were 97.92-100.48%.     

Automatic potentiometric flow titration procedure for ascorbic acid determination in pharmaceutical formulations

A flow procedure for the determination of ascorbic acid in pharmaceutical formulations exploiting potentiometric titration is described. The method is based on the reduction of IO₃⁻ by ascorbic acid and the detection was carried out employing a flow-through ion selective electrode for iodide. The flow network controlled by a microcomputer was designed to implement multicommutation for ease of operation and robustness. The titration system allowed the determination of ascorbic acid in pharmaceutical formulations with concentrations ranging from 7.5 to 15.0 mmol l⁻¹. No significant differences at the 95% confidence level were observed in comparison with results obtained by a manual procedure. Merit figures of results such as a relative standard deviation of 1.0% (n=6) and a reagent consumption of 21.4 mg IO₃⁻ per determination were obtained.     

紫外分光光度法和高效液相色谱法测定淫羊藿总黄酮含量的比较研究

目的:比较紫外分光光度法和高效液相色谱法测定淫羊藿总黄酮含量的差异,探讨淫羊藿总黄酮含量测定方法的可靠性。方法:紫外分光光度法以淫羊藿苷为指标性成分,在270 nm 波长处进行测定。高效液相色谱法以 ZORBAX SB-C_(18)柱(250mm×4.6 mm,5μm)为分析柱,乙腈-水梯度洗脱,流速1.0 mL·min~(-1),检测波长为270 nm。经紫外光谱识别的黄酮类成分(部分经 ESI-MS 确认),除朝藿定 C、淫羊藿苷、鼠李糖基淫羊藿次苷-Ⅱ和宝藿苷Ⅰ以自身对照外,其他黄酮类成分均以淫羊藿苷为参比进行定量,淫羊藿总黄酮含量等于朝藿定 C、淫羊藿苷、鼠李糖基淫羊藿次苷-Ⅱ、宝藿苷Ⅰ和其他黄酮成分含量之和。结果:紫外分光光度法,淫羊藿苷在2.45～24.50μg·mL~(-1)范围内线性关系良好(r=0.9996),测得淫羊藿总黄酮含量以淫羊藿苷计为56.6%。高效液相色谱法中,与淫羊藿苷紫外光谱相似的33个色谱峰,MS 归属了其中10个主要成分均为黄酮类成分。朝藿定 C、淫羊藿苷、鼠李糖基淫羊藿次苷-Ⅱ和宝藿苷Ⅰ分别在0.093～1.852μg(r=0.9998)、0.107～2.136μg(r=0.9997)、0.094～1.876μg(r=0.9998)、0.098～1.956μg(r=0.9998)线性关系良好,淫羊藿总黄酮含量为35.6%。结论:紫外分光光度法和高效液相色谱法测定的淫羊藿总黄酮含量差异显著,紫外分光光度法的准确性有待进一步考证。     

卵磷脂络合碘的制备及电位法测定碘的含量

目的:合成了卵磷脂络合碘,并建立一种以电位滴定法测定卵磷脂络合碘中碘含量的方法.方法:以卵磷脂和碘为原料,乙醚为反应溶剂,三者混合并充分搅拌,回收乙醚得卵磷脂络合碘.采用氢氧化钾乙醇溶液(v/v,1∶5)回流,水解卵磷脂络合碘,以 0.05 mol·L-1硝酸银为标准溶液进行滴定,用电位变化判断滴定终点,从而测定其中碘的含量.结果与结论:合成方法简单,收率高(>96%),合成工艺中使用的乙醚可回收使用,无污染.所建立的电位滴定法测定卵磷脂络合碘中碘的含量,滴定突跃明显,平均回收率为100.1%(RSD为0.21%),精密度RSD为0.34%(n＝6),结果令人满意.     

Validation of HPLC and UV spectrophotometric methods for the determination of meropenem in pharmaceutical dosage form

A high-performance liquid chromatographic method and a UV spectrophotometric method for the quantitative determination of meropenem, a highly active carbapenem antibiotic, in powder for injection were developed in present work. The parameters linearity, precision, accuracy, specificity, robustness, limit of detection and limit of quantitation were studied according to International Conference on Harmonization guidelines. Chromatography was carried out by reversed-phase technique on an RP-18 column with a mobile phase composed of 30 mM monobasic phosphate buffer and acetonitrile (90:10; v/v), adjusted to pH 3.0 with orthophosphoric acid. The UV spectrophotometric method was performed at 298 nm. The samples were prepared in water and the stability of meropenem in aqueous solution at 4 and 25 °C was studied. The results were satisfactory with good stability after 24 h at 4 °C. Statistical analysis by Student's t-test showed no significant difference between the results obtained by the two methods. The proposed methods are highly sensitive, precise and accurate and can be used for the reliable quantitation of meropenem in pharmaceutical dosage form.     

紫外分光光度法测定桂利嗪片含量

本文用紫外分光光度法测定桂利嗪片剂的含量,并与药典方法——非水滴定法进行了比较。结果表明,用紫外分光光度法测定桂利嗪含量,方法简便,其浓度在4～16μg/ml 范围内呈线性关系,r=0.9999,平均回收率为99.78%,与非水滴定法比较,结果基本一致。     

HPLC法和UV分光光度法测定阿奇霉素片溶出度的方法比较

目的采用HPLC和UV分光光度法测定阿奇霉素片溶出度,并从中选择适宜的方法。方法高效液相色谱法,采用ODS-50色谱柱,流动相为0.04M磷酸盐缓冲液(pH 11.0)-乙腈(400∶600),检测波长215 nm,柱温40℃,进样量20μL,溶出介质为磷酸盐缓冲液(pH6.5),转数为75 r/min,45 min取样。紫外分光光度法以磷酸盐缓冲液(pH6.0)为空白溶液及溶剂,检测波长为(482±2)nm,溶出介质为磷酸盐缓冲液(pH6.0),转速为100 r/min,45 min取样。结果溶出曲线方程式为:Y=0.001 3X+0.913,10 min时累计溶出量为92.3%(RSD=1.9%)。回归方程:A=0.007 5C-0.017 1,r=0.999 1。线性范围在17.9~89μg/mL,回收率为99.6%(RSD=0.4%)。结论两种方法都较为准确、简便,测得的溶出效果较好,溶出度结果也基本一致。     

HPLC和络合-UV法测定特非那丁颗粒剂的含量

目的：用ＨＰＬＣ和电荷转移络合ＵＶ法分别测定特非那丁粒剂的含量,并对测定结果进行比较,方法：ＨＰＬＣ法,色谱柱：ＳｐｈｅｒｉｓｏｒｂＣ８（１５０＊４．６ｍｍ,５μｍ）;流动相：甲醇－０．１ｍｏｌ／Ｌ三乙胺磷酸缓冲液（８０：２０）,检测波长２３５ｎｍ。电荷转移络合ＵＶ法,利用碘与ＴＦＮ在氯仿中形成电荷转移络合物的原理,在紫外２９４ｎｍ的波长处测定ＴＦＮ的含量。结果：两法测定的线性范围和平均回收率分别     

HPLC和UV法测定氧氟沙星注射液药物含量的比较

目的 比较HPLC和UV法测定氧氟沙星注射液的含量。方法 采用HPLC法，以氧氟沙星为对照品，检测波长为293nm，甲醇：枸橼酸（0．05mol／L）：乙腈：醋酸铵溶液（0．05mol／L）：10g／L磷酸（100：75：22：1：2）为流动相；采用UV法：用0．1mol／L盐酸作溶剂，测定波长293nm，吸光系数为927。结果 HPLC法的平均回收率为99．44％，RSD为0．83％；UV法测得平均回收率为97．96％，RSD 1．31％。结论 HPLC法结果准确，精密度、重现性均好，与UV法比较有显著性差异（P〈0．05）；HPLC法可替代UV法作为该制剂的含量测定。     

HPLC法和UV法测定加替沙星注射液含量的比较

目的建立HPLC法和UV法测定加替沙星注射液的含量,并比较两法测定结果的差异。方法HPLC法以Nova-pak C18(3.9mm×150mm,4μm)柱分离,甲醇-磷酸盐缓冲液-三乙胺(35∶65∶0.008,pH5.0)为流动相,流速0.9mL.min-1,检测波长293nm;UV法以0.9%氯化钠注射液为溶媒,测定波长均为293nm,吸光系数E11c%m为451。结果HPLC法在10~200μg.mL-1浓度范围线性关系良好(r=0.9997,n=6),平均回收率99.9%,日内及日间RSD<1.04%;UV法线性范围3~40μg.mL-1(r=0.9993,n=6),平均回收率101.1%,日内及日间RSD<1.78%。结论HPLC法与UV法在测定加替沙星氯化钠注射液含量时准确度和精密度无显著差异(P>0.1),均可用于该制剂质量控制。     

头孢呋辛酯片含量测定的不同方法比较

目的 :比较头孢呋辛酯含量测定的 3种不同方法。方法 :分别采用 2种高效液相色谱法 (美国药典XXⅣ版方法、中国药典 2 0 0 0年版方法 )及紫外分光光度法测定头孢呋辛酯片的含量。结果 :3种方法测定头孢呋辛酯片的回收率分别为 99.2 0 % ,99.98%和 99.4 8% ;RSD分别为 1.13% ,1.74 %和 0 .89%。结论 :3种方法均可作为头孢呋辛酯片的含量测定方法。     

紫外分光光度法测定尿素乳膏中尿素的含量

目的：建立紫外分光光度法测定尿素乳膏中尿素的含量。方法：以对一二甲氨基苯甲醛为显色剂,用紫外分光光度计在420nm处测定吸光度。结果：尿素含量在15—120μg／ml范围内具有良好的线性关系（r=0．9998）,平均回收率为99．2％（n=9）,RSD为0．7％,重复性试验RSD为0．3％（n=6）。结论：本方法简便,结果准确可靠,重现性好,可作为控制该制剂质量的主要方法。     

HPLC methods for choloroquine determination in biological samples and pharmaceutical products

ObjectiveReview and assess pharmaceutical and clinical characteristics of chloroquine including high-performance liquid chromatography (HPLC)-based methods used to quantify the drug in pharmaceutical products and biological samples.Evidence acquisitionA literature review was undertaken on the PubMed, Science Direct, and Scielo databases using the following keywords related to the investigated subject: ‘chloroquine’, ‘analytical methods’, and ‘HPLC’.ResultsFor more than seven decades, chloroquine has been used to treat malaria and some autoimmune diseases, such as lupus erythematosus and rheumatoid arthritis. There is growing interest in chloroquine as a therapeutic alternative in the treatment of HIV, Q fever, Whipple’s disease, fungal, Zika, Chikungunya infections, Sjogren’s syndrome, porphyria, chronic ulcerative stomatitis, polymorphic light eruption, and different types of cancer. HPLC coupled to UV detectors is the most employed method to quantify chloroquine in pharmaceutical products and biological samples. The main chromatographic conditions used to identify and quantify chloroquine from tablets and injections, degradation products, and metabolites are presented and discussed.ConclusionResearch findings reported in this article may facilitate the repositioning, quality control, and biological monitoring of chloroquine in modern pharmaceutical dosage forms and treatments.Graphical abstract      

多虑平乳膏的研制及其含量测定

多虑平乳膏神厥穴贴敷治疗各型荨麻疹具有特效。本文报道了多虑平乳膏的制备工艺,选用非离子型表面活性剂吐温80作乳化剂,氮酮作透皮吸收促进剂,经两年多时间观察,乳膏质量稳定,采用紫外分光光度法测定本品的含量,操作简便,快速,平均回收率为99.35%,变异系数为0.5%。     

紫外分光光度法测定金莲花口服液含量

目的建立金莲花口服液中黄酮类物质的含量测定方法。方法采用紫外分光光度法,通过紫外扫描确定最大吸收波长,在最大吸收波长处以芦丁为对照品测量吸光度制定标准曲线,并进行样品溶液稳定性试验、重现性试验、精密度试验、回收率试验等。结果精密度试验所测得的吸光度分别为:0.235、0.234、0.234、0.234、0.233,相对标准偏差(RSD)=0.30%,数据表明该试验具有良好的精密度;稳定性试验测定在0、5、10、15、20、25min时吸光度分别为0.249、0.249、0.248、0.245、0.245、0.244,RSD=0.83%,数据表明在25min内对待测物进行吸光度的测定是稳定的;重现性试验在500nm波长处测定吸光度为:0.412、0.411、0.413、0.407、0.407,RSD=0.69%,表示重现性良好;回收率试验测定的平均回收率为98.5%,RSD=0.56%;样品含量的测定测定的3种批号样本的平均含量分别为0.334mg/ml、0.412mg/ml、0.375mg/ml。结论紫外分光光度法简单方便、准确可靠,可以用来测定金莲花口服液中黄酮类物质的含量。     

Comparison of two derivative spectrophotometric methods for the determination of alpha-tocopherol in pharmaceutical preparations

Simple, sensitive and reliable derivative spectrophotometric methods were developed and validated for determination of alpha-tocopherol in pharmaceutical preparations. The solutions of standard and the sample were prepared in absolute ethanol. The quantitative determination of the drug was carried out using the first derivative values measured at 284, 304 nm and the second derivative values measured at 288, 296 nm. Calibration graphs constructed at their wavelengths of determination were linear in the concentration range of alpha-tocopherol using peak to zero 10-250 microg ml(-1) for first and second derivative spectrophotometric methods. Developed spectrophotometric methods in this study are accurate, sensitive, precise, reproducible, and can be directly and easily applied to Evon dragee form as pharmaceutical preparation. Statistical analysis (Student's t-test) of the obtained results showed no significant difference between the proposed two methods.     

盐酸吗啉胍片含量测定方法的研究

目的：对盐酸吗啉胍片中盐酸吗啉胍的含量测定法进行了比较,方法：分别采用紫外分光光度法、非水滴定法对数家药厂盐酸吗啉胍片的含量测定进行了研究。结果：紫外分光光度法线性关系良好,回收率为99．9,RDS为0．31％,结论：紫外分光光度法优于非水滴定法,该法简便、准确。     

UV法和HPLC法测定盐酸雷尼替丁氯化钠注射液的含量

目的建立了紫外光谱法(UV)和高效液相色谱法(HPLC)测定盐酸雷尼替丁氯化钠注射液的含量.方法UV法用水作溶剂,选择314±2nm作为测定波长;HPLC法用50%甲醇作溶剂,以Alltima C18作为色谱柱,0.1mol/L醋酸钠-甲醇(32∶68)为流动相,流速0.5ml/min,检测波长为320nm.结果UV法盐酸雷尼替丁在4～20μg/ml之间线性良好,相关系数r＝0.99998,回收率为99.8%,RSD＝0.3%(n＝5);HPLC法盐酸雷尼替丁在100～300μg/ml之间线性良好,相关系数r＝0.9998,回收率为100.8%,RSD＝0.4%(n＝5),日内、日间精密度(RSD)分别为0.5%(n＝5)和0.9%(n＝4).结论用上述两法测定本品含量,结果基本一致.     

大孔树脂紫外分光光度法测定皮炎宁中醋酸地塞米松含量

目的 :建立医院制剂皮炎宁的含量测定方法。方法 :采用D 1 0 1大孔树脂分离纯化、紫外分光光度法测定皮炎宁中醋酸地塞米松的含量。结果 :平均回收率为 99.7% ,RSD =1 .2 1 %。结论 :该法简便、快速、准确、重现性好 ,对医院制剂快速分析很适用     

Analysis of miconazole and econazole in pharmaceutical formulations by derivative UV spectroscopy and liquid chromatography (HPLC)

Methods based on derivative UV spectrophotometry and high-performance liquid chromatography (HPLC) have been developed for the selective determination of miconazole and econazole in pharmaceutical dosage forms. A solid-phase extraction (SPE) procedure using a diol column gave quantitative drug extraction from formulated creams and provided purified sample solutions suitable for assay by the derivative UV spectrophotometric and HPLC methods. The proposed methods gave comparable accurate results, whereas a conventional UV spectrophotometric method was found to be seriously affected by excipients.