反相高效液相色谱法同时测定法莫替丁及其相关物质的含量

１　引　言 法莫替丁（famotidine)是日本山之内制药株式会社开发的继西咪替丁、雷尼替丁后的第三代组胺受体拮抗剂,其抑制胃酸分泌比前两者强而持久。日本药典、美国药典及我国部颁标准规定以高氯酸非水滴定法测定其含量;对其相关物质采用薄层色谱法（ＴＬＣ）。此类法定方法的测定准确度及重现性不甚理想,为此,关衍军等对我国部颁标准作了改进;李思明等曾报道了其片剂的紫外分光光度法,沈向忠等用高效液相色谱法（ＨＰＬＣ）测定了其片剂,但都无涉及其原药与相关物质的检测方法。本文研究了法莫替丁原药及其相关物质在ＲＰ－ＨＰＬ…     

Determination of Repertaxin Enantiomeric Purity by HPLC on Chiral Stationary Phase

A precise and sensitive LC method for the determination of repertaxin enantiomeric purity has been developed and validated. Baseline separation with a resolution higher than 2.0 was accomplished within 20 min using a Chiralpak AD-H column (250 × 4.6 mm; particle size 5 μm) and n-hexane:2-propanol (90:10 v/v) as mobile phase at a flow rate of 1 mL min⁻¹. Eluted analytes were monitored by UV detection at 260 nm. The effects of mobile phase composition, temperature and flow rate on enantiomeric selectivity and on resolution of enantiomers were investigated. Calibration curves were plotted within the concentration range between 0.002 and 1.0 mg mL⁻¹ (n = 3), and relative standard deviation (RSD) of the inter-batch assay and intra-batch assay was less than 1.27 and 1.16 %. LOD and LOQ for repertaxin were 0.65 and 2.19 μg mL⁻¹; those for its enantiomer were 0.70 and 2.34 μg mL⁻¹, respectively. The method was evaluated and validated by analysis of bulk samples of repertaxin of different enantiomeric purity. It was demonstrated that the method was accurate, robust, and sensitive, and enabled practical analysis of real samples.

     

反相高效液相色谱法测定泼尼松龙磷酸钠原料药及其注射液

泼尼松龙磷酸钠（prednisolone sodium phosphate,PPNa）为11β,17α,21-三羟基孕甾-1,4-二烯-3,20-二酮-21-磷酸酯二钠盐。目前国内还未上市销售,也无其分析方法的报道,但有对醋酸泼尼松龙进行分析的报道。美国药典26对其提取分离后用紫外分光光度法检测PPNa中的游离泼尼松龙,但对其注射液未做有关物质的测定;英国药典2002年版采用高效液相色谱法检测PPNa原料中的有关物质,流动相系统复杂。本文建立的反相高效液相色谱法。流动相系统简单。能将供试品中的主峰与杂质峰完全分离,方法快速灵敏、准确度高、重复性好,可用于PPNa原料药及其注射剂的含量测定和有关物质的测定。     

Determination and Quantification of Pitavastatin Calcium in Tablet Dosage Formulation by HPTLC Method

Abstract

A simple, sensitive, reliable, and rapid HPTLC method has been developed for the determination of pitavastatin calcium in tablet dosage form. Identification and determination were performed on aluminum backed silica gel 60F₂₅₄ washed with methanol. The mobile phase of ethyl acetate‐methanol‐ammonia‐1 drop formic acid (7:2:0.8) calibration plots were established showing the dependence of response (peak area) on the amount chromatographed. The spot were scanned at 245 nm. The method has a linear range of 50–250 ng/spot. The method was validated for selectivity, repeatability, and accuracy. The method was used for determination of the compound in commercial pharmaceutical dosage forms. It is a more effective option than other chromatographic techniques in routine quality control.     

高效液相色谱法检测替拉扎明中的有关物质

替拉扎明（TPZ）是一种肿瘤放疗增敏剂,其中已知杂质SR4317为TPZ的合成中间体,SR4330为TPZ的可能降解物。TPZ中有关物质的检测目前尚未见文献报道。本文建立的检测TPZ中有关物质的高效液相色谱法（HPLC）,准确、灵敏、快速,可用于TPZ原料药的质量控制。     

反相高效液相色谱法测定硝酸咪康唑及其相关物质的含量

在LUNAC18色谱柱(250×4.6mmI.D,5μm)上,研究了硝酸咪康唑(Mi conazoleNitrate)及其相关物质(Alpha (2,4 Dichlorophenyl) 2 1H Imidazole 1 Ethanol)的反相高效液相色谱分离检测的最适宜条件,采用乙腈∶缓冲溶液=70∶30(V/V)为流动相,流速为1.0mL/min,检测波长为235nm,经实际样品测定,结果满意。这为跟踪产品的合成工艺,提高产品的质量提供了一个快速有效的检测方法。     

System Maps for Retention of Small Neutral Compounds on a Superficially Porous Ethyl-Bridged,Octadecylsiloxane-Bonded Silica Stationary Phase in Reversed-Phase Liquid Chromatography

The system constants of the solvation parameter model are used to prepare system maps for the retention of small neutral compounds on an ethyl-bridged, ocatadecylsiloxane-bonded superficially porous silica stationary phase (Kinetex EVO C18) for aqueous mobile phases containing 10–70% (v/v) methanol or acetonitrile. Electrostatic interactions (cation-exchange) are important for the retention of weak bases with acetonitrile–water but not methanol–water mobile phase compositions. Compared with a superficially porous octadecylsiloxane-bonded silica stationary phase (Kinetex C18) with a similar morphology but different topology statistically significant differences in selectivity at the 95% confidence level are observed for neutral compounds that vary by size and hydrogen-bond basicity with other intermolecular interactions roughly similar. These selectivity differences are dampened with acetonitrile–water mobile phases, but are significant for methanol–water mobile phase compositions containing <30% (v/v) methanol. A comparison of a totally porous ethyl-bridged, octadecylsiloxane-bonded silica stationary phase (XBridge C18) with Kinetex EVO C18 indicated that they are effectively selectivity equivalent.     

磺胺二甲嘧啶及有关物质HPLC检测方法验证

建立了磺胺二甲嘧啶及其可能存在的5种杂质成分:对氨基苯磺酸、4,6-二甲基-2-羧基嘧啶、磺胺脒、磺胺和2-氨基-4,6-二甲基嘧啶的高效液相色谱分离和定量分析方法.采用C18色谱柱,pH 4.0的乙腈-醋酸(体积比1:9)流动相,分离有关杂质,而水-乙腈-冰醋酸(体积比87:12:1)流动相用于主成分磺胺二甲嘧啶(SM2)含量的测定;二极管阵列检测器,检测波长275 nm.上述5种杂质的检出限分别为0.023、0.023、0.009、0.009、0.030 mg/L,满足测定要求.     

HPLC Method for Determination of 3,4-Diaminopyridine in the Presence of Related Substances and Degradation Products Formed Under Stress Conditions

3,4-Diaminopyridine is used to treat some symptoms met in Lambert Eaton myasthenia syndrome. It was shown efficient to reduce a form of variable muscle weakness and fatigability typical of the disease and correlated to a block of acetylcholine release. A high performance liquid chromatographic method for the determination of 3,4-diaminopyridine in the presence of related substances and its degradation products is described. The method is based on the use of a C18 bonded phase column and a mobile phase composed of 10 volumes of acetonitrile and 90 volumes of an aqueous solution containing 1 g L^?1 sodium octanesulfonate and 0.77 g L^?1 ammonium acetate. The pH of the aqueous solution was adjusted to 1.9 with trifluoracetic acid. All peaks are eluted in <40 min. The method was demonstrated to be precise, accurate and specific even though a major part of the drug is decomposed. The results indicate that the proposed method could be used in stability assays.     

高效液相色谱法测定恩替卡韦口服液中有关物质

建立了测定恩替卡韦口服液中有关物质的高效液相色谱法。采用Agilent ZORBAX SB-C18色谱柱,以水-乙腈-三氟乙酸(97∶3∶0.15,V/V)/乙腈为流动相,梯度洗脱,二极管阵列检测器(DAD)检测。杂质A、B和C的检测限分别为7.22ng/mL、7.30ng/mL和7.50ng/mL,分别相当于恩替卡韦浓度的0.014%、0.015%、0.015%;杂质A在24.08~361.0ng/mL浓度范围内(r=0.9988),杂质B在24.33~364.9ng/mL浓度范围内(r=0.9996),杂质C在25.00~375.0ng/mL浓度范围内(r=0.9984)呈现良好的线性关系;在0.125、0.25、0.37μg/mL三个浓度的添加水平下,杂质A、B、C的平均回收率分别为121.9%、115.5%和106.9%。     

氧化型谷胱甘肽二钠及其有关物质的高效液相色谱分析

为考察不同色谱条件下氧化型谷胱甘肽二钠及有关物质的色谱行为,建立了氧化型谷胱甘肽二钠有关物质及含量测定的高效液相色谱分析方法,固定相为Zorbax XB—C18（4．6mm×250mm,5μm）;流动相为V（0．006mol／L辛烷磺酸钠）＋y（甲醇）=95＋5;检测波长为210nm,柱温30℃。结果表明,氧化型谷胱甘肽二钠的线性范围为0．5～10μg,r=0．9999,总有关物质含量小于1．2％。此法简单,分离度良好,结果准确,可以用于氧化型谷胱甘肽二钠的含量测定和有关物质的检测。     

脱叔丁基杯[8]芳烃键合固定相的制备及其液相色谱性能

杯芳烃(Cahixarenes)是一类由苯酚单元经亚甲基相连而成的大环化合物,与β-环糊精类似,它能与多种溶质形成主客体包容配合物,并通过超分子作用识别离子和中性分子等客体,利用杯芳烃的分子识别作用可提高色谱分离性能,Glennon等制备了酯化杯[4,6]芳烃键合固定相,     

A Novel Ultra-High Performance Liquid Chromatography Method for the Determination of Erdosteine,Related Impurities and Degradation Products in New Effervescent Tablets

A novel and automated, stability-indicating, reversed phase ultra performance liquid chromatography (UPLC) method was developed and validated for the quantitative determination of erdosteine, its known impurities and two novel degradation products in a new pharmaceutical dosage form (effervescent tablets). The chromatographic separations were performed on a Waters Acquity UPLC HSS T3, 1.8 µm (2.1 mm?×?150 mm, I.D.) stainless steel column. The mobile phase consisted of 0.1% TFA in water and methanol under gradient elution conditions, at a flow rate of 0.29 mL/min, for the assay and impurities analysis. UV detection was set at a wavelength of 238 nm. Erdosteine raw material, placebo and effervescent tablets were subjected to forced degradation. The new degradation products (labeled OX1 and OX2) were found after oxidative treatment and characterized by ultra performance liquid chromatography mass spectrometry. The validation parameters such as linearity, limit of detection (LOD) and quantification (LOQ), accuracy, precision, specificity and robustness were highly satisfactory for all analyzed compounds. LOD (0.020 and 0.011–0.385 µg/mL for erdosteine and impurities, respectively) and LOQ values show the high sensibility of the method. Specificity of the method was confirmed by testing the matrix components. The validated method demonstrated to be suitable for routine quality control purposes and for routine stability studies of erdosteine in effervescent formulations.     

反相高效液相色谱法测定盐酸齐拉西酮及有关物质

建立了盐酸齐拉西酮及有关物质的反相高效液相色谱测定法。采用C18色谱柱,以甲醇-50mmol／L醋酸钠缓冲溶液梯度洗脱,使盐酸齐拉西酮及8个中间体基线分离,采用二极管阵列检测器,检测波长254砌。各杂质的最低检出限均可满足测定的要求。建立的方法操作简便,重现性好,结果准确。     

HPLC法测定丙酮酸钙的含量

建立一种用高效液相色谱法(HPLC法)测定丙酮酸钙含量的方法。色谱条件为C18柱,乙腈—0.1%二环已胺和0.1%甲酸的水溶液(5:95)为流动相, 检测波长为230nm。线性范围0.08~0.8mg/mL(r = 0.9999)。     

Simultaneous Determination of Cimetidine and Related Compounds in Pharmaceuticals by HPLC on a Porous Graphitic Carbon Column

A high-performance liquid chromatographic method has been developed for determination of cimetidine and its main related compounds, 4-hydroxymethyl-5-methylimidazol (MH), N-cyano-N',N''-dimethylguanidine (Carbonate), 1-methyl-3-[2-[[(5-methyl-1H-imidazol-4-yl)methyl]sulfonyl]ethyl]guanidine (Guanidine), 2-cyano-1-methyl-3-[2-[[(5-methyl-1H-imidazol-4-yl)methyl]sulfonyl] (Sulfoxide), and 1-[(methylamino)[[2-[[(5-methyl-1H-imidazol-4-yl)methyl]sulfonyl]ethyl]amino]methylene]urea (Amide). Chromatographic separation was achieved on a porous graphitic carbon (PGC) column with a gradient 17:83 to 19:81 (v/v) acetonitrile-0.05 M potassium phosphate buffer containing 0.40% pentane sulfonic acid at pH 2.5. Analysis was performed at a flow-rate of 1 mL min^?1 and the detection wavelength was 228 nm. Calibration plots were linear in the concentration ranges 0.25 to 83 µg mL^?1 for cimetidine and Carbonate, 0.25 to 75 µg mL^?1 for Guanidine, Amide, and Sulfoxide, and 0.25 to 100 µg mL^?1 for MH, with correlation coefficients (R ²) between 0.9990 and 0.9998. The lowest detectable concentration of cimetidine and Amide was 0.07 µg mL^?1; for MH, Carbonate, Guanidine, and Sulfoxide it was 0.06 µg mL^?1. Method repeatability (intraday) and reproducibility (interday) was always less than 2% (n=5). The proposed liquid chromatographic method was successfully used for analysis of commercially available cimetidine dosage forms; recoveries were from 99.2 to 100.8%.     

高效液相色谱手性固定相法拆分四面体金属簇合物

在正相条件下,在Ch iralpak(AD-H和Ch iralcel(OD-H两种手性色谱柱上,首次直接拆分了三种外消旋过渡金属簇合物,考察了流动相中极性添加剂醇对手性拆分的影响.结果发现,氢键作用在手性识别过程中起重要作用,而且不同的色谱柱填料有不同的选择性.