磷酸氯喹中有关杂质的分析

采用ＧＣ、ＴＬＣ、ＧＣ－ＭＳ联用技术，分离和确证了磷酸氯喹中的有关杂质为５－氯和其它的同分异构体以及脱乙基物     

硫酸卡那霉素及其注射液的HPLC衍生化测定

以异硫氰酸苯酯（ＰＩＴＣ）为衍生试剂，用柱前衍生化反相ＨＰＬＣ分离测定硫酸卡那霉素及其注射液。对杂质卡那霉素Ｂ采用归一化法进行了检查。     

反相快速HPLC测定核糖霉素方法的研究

本文选用３，５－二硝基苯甲酰氯作衍生化试剂，柱前衍生，采用二极管阵列紫外检测器检测，研究并建立了核糖霉素及杂质新霉胺的反相快速ＨＰＬＣ测定方法。采用高效细颗粒短柱进行分离，整个分析时间少于５ｍｉｎ，实现了高效快速测定。     

反相HPLC法测定先锋霉素Ⅳ胶囊和片剂的含量

采用反相ＨＰＬＣ法测定先锋霉素Ⅳ胶囊及片剂中先锋霉素Ⅳ含量。采用Ｃ１８Ｈｙｐｅｒｓｉｌ色谱柱，甲醇－ＨＡＣ－ＮａＡＣ缓冲液作流动相，检测波长２５４ｎｍ。方法简便，专一性强，制剂辅料及原料药中有关杂质不影响测定，两种制剂的回收率分别为９８．１３－１０１．３％和９８．２２－１０２．５％，ＲＳＤ＜２．７％（ｎ＝５）．     

抗孕唑注射液及其相关物质的反相高效液相色谱分析法

本实验建立了反相ＨＰＬＣ法测定终止早孕新药抗孕唑（ＤＬ１１１－ＩＴ）注射液的含量及其相关物质检查的方法。采用ＳｈｉｍｐａｃｋＯＤＳ柱，以炔诺酮为内标，甲醇－水７：３（ｐＨ７．５）为流动相，检测波长２４０ｎｍ，测得线性范围２～１００μｇ／ｍｌ（ｒ＝０．９９９９），平均回收率１００．３％，ＲＳＤ为１．０２％。分析了注射液中可能存在的相关杂质及影响因素。最小检出量为１４．３２ｐｍｏｌ。此法简便、专属、准确，可同时进行含量测定与杂质检查。     

HPLC在有关物质检查中的应用探讨

杂质检查是药品质量标准的重要组成部分 ,对一些特殊杂质的控制 ,既能保证用药的安全有效 ,又能考核药物的生产工艺和贮存条件。本文就ＨＰＬＣ在有关物质检查中遇到的一些问题与同行进行探讨 ,旨在提高检测水平 ,加强药品的质量控制。(1)在药品检验中ＨＰＬＣ的检测器应用最多的是选择型紫外检测器。为了获得最大的灵敏度和抗干扰能力 ,一般都选择欲分析物质有最大吸收的波长进行检测 ,即测定波长的选择取决于待测物质的组成和结构。在药品标准中有关物质的检查多采用与主成分测定相同的检测波长 ,而此时应主要考虑杂质的响应因子 ,由此可…     

瑞巴派特的HPLC测定

采用ＨＰＬＣ测定瑞巴派特含量及其杂质。色谱柱为ＹＷＧＣ１８,流动相为甲醇－ＰＨ６．５磷酸盐缓冲液（含１％氢氧化四丁基铵的１０％水溶液（５２：４８）。方法简便、结果准确。     

甲硝唑及注射液中有关物质的测定及稳定性的初步研究

目的：采用高效液相色谱法测定甲硝唑原料及注射液中的有关物质,并初步考察其稳定性。方法：以国产ＹＷＧ－Ｃ１８１０μｍ１５０ｍｍ×４６ｍｍ色谱柱为分析柱,以乙腈－水（８５∶９１５）为流动相,柱温２５℃,检测波长２２５ｎｍ,以峰面积归一化法处理结果。结果：原料药可分离２个杂质峰,注射剂可分出３个杂质峰,强光照射注射液可使一杂质峰显著增加。结论：本法简便、快速、准确,可作为样品中杂质的检测方法。     

药典采用高效液相色谱法控制药物杂质限量方法的讨论

药典采用高效液相色谱法控制药物杂质限量方法的讨论张启明（中国药品生物制品检定所北京１０００５０）《中国药典》自１９７７年版在检查药物有机杂质时开始使用薄层色谱法（ＴＬＣ），随着高效液相色谱（ＨＰＬＣ）方法的普及，《中国药典》自１９９０年版有部分品种采...     

葡萄糖注射液中5—羟甲基糠醛检查的实验考查

葡萄糖注射液中５—羟甲基糠醛检查的实验考查王荣（山东省枣庄市药品检验所２７７１４７）５—羟甲基糠醛（５—ＨＭＦ）是葡萄糖制剂中含有的一种有害杂质，《中国药典》１９８５年版、１９９０年版均规定了对葡萄糖注射液和葡萄糖氯化钠注射液进行５—ＨＭＦ的检查。在...     

Structural studies of racecadotril and its process impurities by NMR and mass spectroscopy

Three unknown impurities in racecadotril bulk drug at levels below 0.5% were detected by simple reverse phase isocratic high performance liquid chromatography (HPLC). Structures for these impurities were proposed by molecular ion information and their fragmentation pattern obtained by LC-MS and these impurities were confirmed by NMR spectroscopy. The impurities I, II and III were characterized as benzyl 2-methyl carboximido acetate, benzyl 2-phenyl ethyl carboximido acetate, and benzyl 2-(1-benzyl vinyl carboximido) acetate. These structures were further confirmed by co-injecting of synthetic standards of impurities with racecadotril. The mechanism of the formation of these process related impurities is discussed.     

己酮可可碱中杂质的反相高效液相色谱检测

以反相高效液相色谱法测定己酮可可碱中的杂质，采用ＯＤＳ柱，以甲醇－水－冰乙酸（４５：５５：５）为流动相，紫外检测波长为２７４ｎｍ，本法比薄层色谱法分离效果好，精密度高，且具有良好重现性。     

Detection, isolation and characterization of principal synthetic route indicative impurities in verapamil hydrochloride

Two unknown impurities were detected in verapamil hydrochloride bulk drug using isocratic reversed-phase high performance liquid chromatography (HPLC). These impurities were isolated by preparative HPLC. Spectral data for the isolated impurities were collected. Based on the spectral data derived from two-dimensional nuclear magnetic resonance (2D-NMR) spectroscopy and mass spectrometry (MS), impurity-1 and impurity-2 were characterized as 2-(3,4-dimethoxyphenyl)-3-methylbut-2-enenitrile and 2-(3,4-dimethoxyphenyl)-2-isopropyl-3-methylbutanenitrile, respectively.     

Isolation and characterization of some potential impurities in ropinirole hydrochloride

Three impurities in ropinirole hydrochloride drug substance at levels approximately 0.06-0.15% were detected by reverse-phase high performance liquid chromatography (HPLC). These impurities were isolated from the drug substance. These impurities were analyzed using reverse-phase HPLC. Based on the spectral data (IR, NMR and MS), structures of these impurities were characterized as 4-[2-(propylamino) ethyl]-1,3-dihydro-2H-indol-2-one hydrochloride (impurity-A), 5-[2-(diropylamino) ethyl]-1,4-dihydro-3H-benzoxazin-3-one hydrochloride (impurity-B) and 4-[2-(diropylamino) ethyl]-1H-indol-2,3-dione hydrochloride (impurity-C). Synthesis of these impurities is discussed.     

LC-MS法分析头孢硫脒中的主要杂质

目的对国内四家头孢硫脒制剂产品进行检测,确证超过报告限度(>0.05%)杂质的结构。方法采用HPLC法、LC-MS法及NMR法对头孢硫脒进行了强制降解杂质研究、长期留样杂质研究、杂质谱研究。结果存在四个超过报告限度的杂质,降解杂质为去乙酰头孢硫脒和头孢硫脒内酯,其他杂质为7-溴乙酰胺头孢烷酸(7-BCA)、头孢硫脒Δ2异构体。结论为头孢硫脒的质量控制和稳定性研究提供了重要依据。     

Isolation and structural elucidation of two impurities from a diacerein bulk drug

Two impurities were found in the crude sample of diacerein. The level of these impurities 1.14% and 1.24% were detected by isocratic reverse-phase high performance liquid chromatography (HPLC). The molecular weights of the impurities were determined by liquid chromatography–mass spectroscopy (LC–MS) analysis. These impurities were isolated from crude sample of diacerein by reverse-phase preparative liquid chromatography. These impurities were characterized as 5-acetoxy-4-hydroxy-9,10-dioxo-9,10-dihydroanthracene-2-carboxylic acid (Impurity-1) and 4-acetoxy-5-hydroxy-9,10-dioxo-9,10-dihydroanthracene-2-carboxylic acid (Impurity-2) respectively. Structural elucidation of both the impurities were carried out by ¹H NMR, ¹³C NMR, DEPT, 1D NOESY, MS and IR spectroscopy.     

氨苄青霉素中致敏性杂质的比较分析及产品致敏性评价方法的建立

溶媒结晶工艺和喷雾干燥工艺生产的氨苄青霉素中致敏性杂质的种类不同。前者主要为非聚合物类杂质,后者含有聚合物类杂质和非聚合物类杂质。豚鼠PCA试验证明两类杂质引发过敏反应的能力和与其作用的氨苄青霉素抗体的匹配程度有关。用凝胶过滤法,对54批国产和进口的氨苄青霉素样品进行了考察。结果表明,各批样品间非聚合物类杂质的含量差异很大。以聚合物类杂质含量和非聚合物类杂质含量二个指标来评价氨苄青霉素的致敏性,在广泛考察样品的基础上,用模式识别(Pattern recognition)法建立了评价商品氨苄青霉素致敏性的数学模型,可以方便地对不同样品的致敏性进行评价、比较。     

Structural studies of impurities of risperidone by hyphenated techniques

During the impurity profile of risperidone (RSP), a more polar impurity (RSP-1) and a more non-polar impurity (RSP-2) were detected in LC-MS with respect to risperidone. These impurities were isolated, enriched and were subjected to mass and NMR spectral studies. Based on the spectral data, RSP-1 and RSP-2 were characterized as risperidone N-oxide and 9-methylene risperidone, respectively. The formation of these impurities is rationalized. The structures of both the impurities were unambiguously confirmed by single crystal XRD Studies.     

褶合光谱法用于DNA样品中杂质的限量检查

目的　对DNA样品中苯酚、氨基酸和内毒素进行限量检测。方法　采用褶合变换技术、光谱空间理论提出的相关系数判别分析法和计算机信息处理技术进行杂质检查。结果　褶合光谱法与二阶导数光谱法及A₂₆₀/A₂₈₀比值法结果相对照。表明本法可对DNA样品中杂质进行半定量检测。结论　本法快速、简便、准确,可用于生化样品分析。     

Identification of gentamicin impurities by liquid chromatography tandem mass spectrometry

An HPLC/MS/MS method was developed for identification of impurities in gentamicin. The HPLC was performed on a Synergy Hydro-RP column using 50 mM trifluoroacetic acid (TFA), pH 2 adjusted with ammonium solution and methanol as mobile phase. All impurities in gentamicin were separated from main gentamicin components. Atmospheric pressure chemical ionization (APCI) was used and product mass spectra of protonated molecules were acquired. Seventeen impurities were detected in gentamicin. Reference compounds: gentamicins: C_2b, B, B₁, G-418, sisomicin, garamine and gentamines: C₁, C_1a, C₂, C_2a were used for spectra interpretation and impurities identification. All MS/MS spectra were interpreted and fragmentation transitions for gentamicins and in general for aminoglycoside antibiotics (AG) were proposed. All impurities were identified. More than one isomere were proposed for three impurities.