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…     

高效液相色谱法和毛细管电泳法测定甘草制品中甘草酸的含量

分别用高效液相色谱法（ＨＰＬＣ）、毛细管区带电泳法（ＣＺＥ）、胶束电动毛细管色谱法（ＭＥＣＣ）测定了甘草制品中甘草酸的含量。对ＨＰＬＣ,ＣＺＥ,ＭＥＣＣ的分析条件作了一些选择实验,结果表明ＭＥＣＣ法与ＨＰＬＣ法分析数据接近、比较准确,而且前者比ＨＰＬＣ法分离效率高、溶剂用量少,是一种很有发展潜力的分析方法。     

反相高效液相色谱法测定染料中间体1,8-二氨基萘

1 ,8 二氨基萘 ( 1 ,8 ｄｉａｍｉｎｏｎａｐｈｔｈａｌｅｎｅ)是一种常用试剂 ,主要作为中间体[1 ] 而用于一些染料的有机合成中。由于 1 ,8 二氨基萘应用极为广泛而配成溶液稳定性较差[2 ] ,给测定其含量带来了一定的困难 ,因此本文就如何在允许的条件下精密测定其含量的方法用高效液相的方法进行了研究 ,提出了一种用ＨＰＬＣ法测定工业产品中 1 ,8 二氨基萘的方法。1　实验部分1 1　仪器与试剂ＬＣ 6Ａ高效液相色谱仪 (日本岛津公司 ) ;Ｃ Ｒ3Ａ数据处理系统 ;ＳＰＤ 6ＡＶ紫外可见分光光度检测器。 1 ,8 二氨基萘标准品和工业产品 (…     

反相高效液相色谱法同时测定发酵乳中的蛋白糖和氨基酸

介绍了同时测定发酵乳中蛋白糖和氨基酸的ＨＰＬＣ方法。样品经甲醇除去蛋白,异硫氰酸苯衍生,ＲＰ－ＨＰＬＣ法测定。蛋白糖回收率为９４．２％～９８．７％,精密度以相对标准偏差表示为２．１５％～３．７４％。     

HPLC检测柑桔类水果中无机溴化合物残留量

采用ＨＰＬＣＳｈｉｍ－ｐａｃｋＩＣ－Ａ１柱，紫外检测器测定柑桔类水果中无机溴残留量，样品经氢氧化钠乙醇溶液水解，灰化后进行ＨＰＬＣ分析。方法简便，重复性好（ＣＶ＝０．９５～８．６１％），样品检出限为１０￣（－６），添加回收大于９０％。     

反相高效液相色谱法测定来氟米特含量及对有关物质的检查

1　引　　言来氟米特 (ｌｅｆｌｕｎｏｍｉｄｅ) ,化学名为Ｎ (4 三氟甲基苯基 ) 5 甲基异唑 4 甲酰胺 ,可用于治疗类风湿性关节炎。该药与非甾体抗炎药 (ＮＳＡＩＤｓ)不同 ,它具有抗增殖和抗炎活性。它能抑制二氢乳酸脱氢酶 ,是嘧啶合成的抑制剂 ,我厂已研制成功该药。文献曾以高效液相色谱法 (ＨＰＬＣ)测定片剂的含量 ,但不能检查其有关物质。本文用ＨＰＬＣ法测定来氟米特含量及对有关物质检查反相高效液相色谱法测定来氟米特含量及对有关物质的检查@姜少灏$河北医科大学制药厂!石家庄050017 @康丽娟$河北医科大学制药厂!石家…     

高效液相色谱法测定强化奶及食品中维生素D含量

介绍用反相高效液相色谱法（ＨＰＬＣ）测定食品中ＶＤ含量,样品经皂化、正己烷提取、正相ＨＰＬＣ净化,用反相ＨＰＬＣ定量分析。回收率为９４．８８％～９９．７０％,批内和批间ＣＶ分别为１．６２％和２．１２％。分析了奶粉、要素膳、肉松、儿保饮料等８种食品中ＶＤ含量,亦可用于各种食品中ＶＤ分析。     

高效液相色谱-间接光度检测法测定体液中西梭霉素

采用高效液相色谱－间接光度检测法（ＨＰＬＣ－ＩＰＤ）,在流动相中加入具有紫外检测响应的检测剂烟酰胺,用紫外检测器直接测定体液中无紫外吸收的西梭霉素含量。固定相为ＳｐｈｅｒｉｓｏｒｂＣ１８,流动相为甲醇－乙腈－水（２０∶１０∶７０）,内含磷酸０．０５ｍｏｌ／Ｌ、烟酰胺０．５ｍｍｏｌ／Ｌ、庚烷磺酸钠５ｍｍｏｌ／Ｌ。血清样品中西梭霉素平均回收率为９６．９２％±４．６３％,日内和日间变异系数分别为４．７５％和５．６５％。     

双波长导数光谱法测定牡丹皮中丹皮酚的含量

1 引言 牡丹皮为毛茛科植物牡丹(Paeonia suffruticosa Andr.)的干燥根皮,是临床常用的一种中药,具有清热凉血、活血化瘀之功效。丹皮酚是其中主要的化学成分,其它成分尚有芍药甙、丹皮甙、挥发油和苯甲酸,植物甾醇等。丹皮酚的含量是评价牡丹皮质量的一个重要指标,中国药典采用水蒸汽蒸馏—紫外法测定其含量。我们采用双波长导数光谱法测定了牡丹皮中丹皮酚的含量,结果较为满意。     

对酞内酰胺苯磺酰氯柱前衍生HPLC法测定仲丁胺残留量

本实验采用对酞内酰胺苯磺酰氯（Ｐｈｔｈａｌｉｍｉｄｙｌ－ｂｅｎｅｚｅｎｅｓｕｌｐｈｏｙｌｃｈｌｏｒｉｄｅ，简称Ｐｈｉｓｙｌ－Ｃｌ）衍生反相ＨＰＬＣ法进行仲丁胺残留分析，以紫外检测器测定，最低检出限６．２ｐｍｏｌ。     

A review of chromatographic methods for determination of synthetic food dyes

The purpose of this work was to present a chromatographic methods to analyse synthetic food dyes. The following techniques has been described: thin-layer liquid chromatography (TLC), high performance thin-layer chromatography (HPTLC), traditional column chromatography, high performance liquid chromatography (HPLC), include: ion-pair chromatography (HPLC IP), reversed phase chromatography (RP HPLC) and high performance ion chromatography.     

Correlation of TLC,HPTLIC and PMD Results and Their Transfer to HPLC Systems

Abstract

The correlation of the results of five thin-layer chromatographic techniques and their transfer to high performance liquid chromatography are reported. The data obtained indicate that high performance thin-layer chromatographic results are faithfully reproduced by high performance liquid chromatography. Although plates were not activated, and mixed solvents were used, no major differences were observed between thin layer and high performance liquid chromatography.     

Off‐line comprehensive two‐dimensional reversed‐phase countercurrent chromatography with high‐performance liquid chromatography: Orthogonality in separation of Polygonum cuspidatum Sieb. et Zucc

Off‐line comprehensive two‐dimensional reversed‐phase countercurrent chromatography with high‐performance liquid chromatography was investigated in separation of crude ethanol extract from traditional Chinese medicinal herb Polygonum cuspidatum Sieb. et Zucc. Two‐dimensional contour plots for countercurrent chromatography with high‐performance liquid chromatography was obtained after comprehensive separation was completed. Total peak capacity was evaluated and approximately 810 peaks were obtained through a comprehensive two‐dimensional separation. A highly orthogonality of 52.23% and a large separation space occupancy of 88.86% were achieved. Meanwhile, it was found that several components could be well separated by countercurrent chromatography while they could not be separated by high‐performance liquid chromatography, and vice versa, which further indicated the orthogonality of the two separation methods. The off‐line comprehensive two‐dimensional countercurrent chromatography with high‐performance liquid chromatography provided a promising and powerful method for separation of complex natural products.     

Comparison of ultra high performance supercritical fluid chromatography,ultra high performance liquid chromatography,and gas chromatography for the separation of synthetic cathinones

A comparison of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography for the separation of synthetic cathinones has been conducted. Nine different mixtures of bath salts were analyzed in this study. The three different chromatographic techniques were examined using a general set of controlled synthetic cathinones as well as a variety of other synthetic cathinones that exist as positional isomers. Overall 35 different synthetic cathinones were analyzed. A variety of column types and chromatographic modes were examined for developing each separation. For the ultra high performance supercritical fluid chromatography separations, analyses were performed using a series of Torus and Trefoil columns with either ammonium formate or ammonium hydroxide as additives, and methanol, ethanol or isopropanol organic solvents as modifiers. Ultra high performance liquid chromatographic separations were performed in both reversed phase and hydrophilic interaction chromatographic modes using SPP C18 and SPP HILIC columns. Gas chromatography separations were performed using an Elite‐5MS capillary column. The orthogonality of ultra high performance supercritical fluid chromatography, ultra high performance liquid chromatography, and gas chromatography was examined using principal component analysis. For the best overall separation of synthetic cathinones, the use of ultra high performance supercritical fluid chromatography in combination with gas chromatography is recommended.     

环境样品中硝基苯类化合物的分析方法研究进展

主要介绍了我国近年来在环境样品中硝基苯类化合物的分析研究进展,内容包括:光度法(还原-偶氮光度法、阻抑动力学光度法、化学计量学分光光度法、人工神经网络-分光光度法)、气相色谱法(固相微萃取-毛细管气相色谱法、树脂吸附-气相色谱法、液-液微萃取气相色谱法、超声萃取-气相色谱法)、高效液相色谱法(反相高效液相色谱法、固相萃取-高效液相色谱法)和极谱法等分析方法。     

Recent advances of online coupling of sample preparation techniques with ultra high performance liquid chromatography and supercritical fluid chromatography

Ultra high performance liquid chromatography and supercritical fluid chromatography techniques are favored because of their high efficiency and fast analysis speed. Although many sample preparation techniques have been coupled with common liquid chromatography online, the online coupling of sample preparation with the two popular chromatography techniques have gained increasing attention owing to the increasing requirements of efficiency and sensitivity. In this review, we have discussed and summarized the recent advances of the online coupling of sample preparation with ultra high performance liquid chromatography and supercritical fluid chromatography techniques. The main sample preparation techniques that have been coupled with ultra high performance liquid chromatography online are solid‐phase extraction and in‐tube solid‐phase microextraction, while solid‐phase extraction and supercritical fluid extraction are the main techniques that have been coupled with supercritical fluid chromatography online. Especially, the strategies for online coupling of sample preparation with chromatography techniques were summarized. Typical applications and growing trends of the online coupling techniques were also discussed in detail. With the increasing demands of improving the efficiency, throughput, and analytical capability toward complex samples of the analysis methods, online coupling of sample preparation with chromatography techniques will acquire further development.     

多维高效液相色谱技术在蛋白质分离研究中的进展

蛋白质组学出现之后,多维高效液相色谱(multidimensional HPLC,MD-HPLC)系统以其快速、高效、自动化程度高以及容易与质谱等其他技术联用等优势而成为蛋白质组学相关分析技术中研究应用的热点。本文主要以本实验室在蛋白质组学研究中的技术进展为主线,介绍了多维高效液相色谱技术的发展,包括经典的“bottom-up”技术和“top-down”式的多维高效液相色谱技术路线,以及为了提高系统的分离通量而自行设计搭建的阵列式多维高效液相色谱平台,这些技术路线在蛋白质组学研究中有着极大的潜在应用价值。     

Separation and purification of two minor typical diarrhetic shellfish poisoning toxins from harmful marine microalgae via combined liquid chromatography with mass spectrometric detection

A novel method was developed for the purification of two typical diarrhetic shellfish poisoning toxins from toxin‐producing marine microalgae using macroporous resin, high‐speed countercurrent chromatography–mass spectrometry, and semipreparative high‐performance liquid chromatography–mass spectrometry. Analytical high‐performance liquid chromatography–mass spectrometry was used for identification and purity analysis of okadaic acid and dinophysistoxin‐1 because they exhibit no visible or ultraviolet absorption. First, four kinds of macroporous resins were investigated, and HP‐20 macroporous resin was selected for the preenrichment and cleanup of the two target toxins. Second, the resin‐purified sample was further purified using high‐speed countercurrent chromatography coupled with a mass spectrometer. The purities of the obtained okadaic acid and dinophysistoxin‐1 were 89.0 and 83.0%, respectively, as determined through analytical high‐performance liquid chromatography–mass spectrometry. Finally, further purification was carried out using semipreparative high‐performance liquid chromatography with mass spectrometry, and the purities of the final okadaic acid and dinophysistoxin‐1 products were both over 98.0% based on the analytical high‐performance liquid chromatography–mass spectrometry chromatograms and fraction spectra. This work demonstrates that the proposed purification process is a powerful method for the preparation of high‐purity okadaic acid and dinophysistoxin‐1 from toxin‐producing marine microalgae. Moreover, it is particularly important for the purification and preparation of minor toxins that exhibit no visible or ultraviolet absorption from harmful marine algae.     

Erratum to: UPLC versus HPLC on Drug Analysis: Advantageous,Applications and Their Validation Parameters

Liquid chromatography (LC) is a separation technique used in many different areas to aid the identification and quantification of substances in various matrices. LC techniques with various detection modes have been widely used for the sensitive and selective determination of trace amounts of pharmaceutical active compounds in biological samples and their dosage forms. A completely new system design with advanced technology has been developed, called ultra high performance liquid chromatography, which has evolved from high performance liquid chromatography. The application of LC methods to drug analysis introduces a powerful tool for therapeutic drug monitoring as well as for clinical research. The advantages of short turnaround time, method reliability, method sensitivity, and drug specificity justify the use of LC techniques for various groups of the drug active compounds. This review describes some of the principles of ultra high performance liquid chromatography and high performance liquid chromatography, validation of these methods, system suitability tests for the methods, and application of methods to pharmaceutical analysis in the last 3 years.

     

UPLC versus HPLC on Drug Analysis: Advantageous, Applications and Their Validation Parameters

Liquid chromatography (LC) is a separation technique used in many different areas to aid the identification and quantification of substances in various matrices. LC techniques with various detection modes have been widely used for the sensitive and selective determination of trace amounts of pharmaceutical active compounds in biological samples and their dosage forms. A completely new system design with advanced technology has been developed, called ultra high performance liquid chromatography, which has evolved from high performance liquid chromatography. The application of LC methods to drug analysis introduces a powerful tool for therapeutic drug monitoring as well as for clinical research. The advantages of short turnaround time, method reliability, method sensitivity, and drug specificity justify the use of LC techniques for various groups of the drug active compounds. This review describes some of the principles of ultra high performance liquid chromatography and high performance liquid chromatography, validation of these methods, system suitability tests for the methods, and application of methods to pharmaceutical analysis in the last 3 years.