高效液相色谱法同时测定复方对乙酰氨基酚片中3组分的含量

目的:建立以高效液相色谱法同时测定复方对乙酰氨基酚片中对乙酰氨基酚、咖啡因、阿司匹林含量的方法。方法:色谱柱为ODS,流动相为甲醇-4.2%的冰醋酸溶液(3∶7),流速为1.0ml/min,检测波长为275nm,进样量为20μl,柱温为25℃。结果:对乙酰氨基酚、咖啡因、阿司匹林的线性范围分别为16.08～428.80μg/ml(r=0.9981)、3.42～91.20μg/ml(r=0.9988)、23.87～769.92μg/ml(r=0.9999),平均回收率分别为99.2%(RSD=0.23%)、100.4%(RSD=0.63%)、99.3%(RSD=0.11%)。结论:本方法简便、快速、准确,可用于复方对乙酰氨基酚片的含量测定。     

高效液相色谱法测定匹林咖敏片中3组分的含量

目的:采用高效液相色谱法同时测定匹林咖敏片中3组分咖啡因、阿司匹林和马来酸氯苯那敏的含量。方法:色谱柱为ZORBAX Eclipse XDB-C_(18)(150mm×4.6mm,5μm),流动相为甲醇-4.3%冰醋酸溶液(17:83),柱温30℃,流速为1.0ml·min~(-1),检测波长为262nm。结果:咖啡因、阿司匹林和马来酸氯苯那敏的线性范围分别为:3.2～50.6μg·ml~(-1)(r=1.000 0)、24.5～392μg·ml~(-1)(r=1.000 0)和0.4～6.6μg·ml~(-1)(r=0.999 9);平均回收率分别为99.2%,99.3%,99.5%,RSD分别为1.1%,0.7%,0.6%。结论:方法快速、简便,适用于控制药品质量。     

胶束电动色谱法同时测定冬凌草片中冬凌草甲、乙素的含量

目的:建立同时测定冬凌草片中冬凌草甲、乙素含量的方法。方法:采用胶束电动色谱法。运行溶液为25mmol.L-1的十二烷基硫酸钠(SDS)Tris缓冲液,电压25kV,检测波长为240nm。结果:冬凌草甲、乙素的线性范围分别为50~300mg.L-1、25~200mg.L-1,平均回收率分别为99.7%,99.6%。结论:该方法准确可靠、方便快捷,能有效地控制药品质量。     

薄层色谱法同时鉴别克感敏片中四组分

克感敏片是一种常用的解热镇痛药,每片含氨基比林０１ｇ,非那西丁０１５ｇ,咖啡因００３ｇ,扑尔敏０００２ｇ,各地方标准均有收载［１,２］,对这４种组分均采用化学反应来进行鉴别,且扑尔敏的反应不专属,已有报道用薄层色谱鉴别咖啡因与扑尔敏［３］。本...     

偏最小二乘紫外分光光度法同时测定克感敏片中三种成分的含量

介绍了偏最小二乘法在分光光度法中同时测定复方药物的原理。用该法对克感敏片中三种成分非那西汀、氨基比林和咖啡因的含量进行了同时测定,所得平均回收率为100.2±0.4%,99.6±0.6%和100.3±0.7%(置信度为95%)。     

HPLC同时测定阿司匹林、乙柳酰胺、咖啡因复方感冒片中三组分的含量

目的：建立同时测定阿司匹林、乙柳酰胺、咖啡因复方感冒片中三组分的含量的高效液相色谱法。方法；利用Inertsil-ODS柱，流动相为甲醇-0．1％二乙胺水溶液-冰醋酸（40：56：4），流速：1．0mL／min，检测波长280nm，外示法计算，结果：线性范围分别是：阿司匹林120～480μg／mL，r=0．9998；乙柳酰胺40～160μg／mL，r=0．9998；咖啡因20～80μg／mL，r=0．9997。回收率：阿司匹林100．3％；乙柳酰胺100．7％；咖啡因99．7％。结论：本方法分离效果好，辅料无干扰，快速，简便，适合于试制剂三组分的同时测定。     

复方阿斯匹林片中二组分的薄层扫描测定

复方阿斯匹林片中含扑热息痛（1）、咖啡因（2）、阿斯匹林三种组分,是常用的解热镇痛药之一。文献报道可用零交导数与多波长系数分光光度法[1]测定其组分的含量。本文采用薄层扫描法在同一薄层板上测定扑热思痛、咖啡因的含量,简便、快速,结果满意。1仪器与试药岛津CS－9301（PC）S薄层扫描仪（日本）;PQB—Ⅰ型薄层自动铺板器;1μl、2μl、3μl、5μl定量毛细管（美国Drummond公司出品）;硅胶GF254（青岛海洋化工厂）。1、2标准品均由中国药品生物制品检定所提供;复方阿斯匹林片（市售品）;试剂均为分析纯。2分析条件的选择2…     

系数倍率法直接测定复方乙酰水杨酸片中三组分的含量

复方乙酰水杨酸片中含有乙酰水杨酸、非那西酊、咖啡因。中国药典(一九九七年版)是采用有机氯仿提取回流、氧化还原反应对三组分分别滴定定     

胶束薄层色谱分离甘草活性成分的影响因素及优化方法

目的:为甘草的胶束薄层色谱指纹图谱寻找最优胶束流动相。方法:首先采用单因子法,寻找影响甘草胶束薄层色谱的影响因素,在此基础上,采用控制加权可变步长单纯形优化法进行甘草胶束薄层色谱指纹图谱的流动相优化。结果:对甘草的胶束薄层色谱分离条件(表面活性剂的种类和含量、醇和酸改性剂的影响等)进行了实验,表明纯胶束薄层色谱的柱效较低,加入醇和酸类改性剂后柱效有明显提高。通过对改性胶束的进一步优化(控制加权可变步长单纯形优化法),得到优化的甘草改性胶束展开剂组成为:0.23 mol.L-1的SDS+16%(v/v)正丁醇+11%(v/v)甲酸。本研究对胶束薄层色谱的一些分离机理亦进行了探讨。结论:胶束薄层色谱的表面活性剂和各添加剂间存在交互作用,需采用合适的优化方法,才能达到分离中药材复杂活性成分群的目的。     

薄层扫描法同时测定Vc银翘片中的3组分含量

目的建立Vc银翘片中扑热息痛、扑尔敏、Vc 3种成分同时定量的分析方法。方法用超声提取 ,以乙酸乙酯∶冰醋酸∶水 (7∶2∶3,V∶V∶V)为展开剂 ,通过双薄层扫描法对Vc银翘片中扑热息痛、扑尔敏和Vc进行同时定量。结果扑热息痛点样量在 10～ 30 μg,扑尔敏在 1～ 3μg,Vc在2 5～ 75 μg呈现良好的线性关系。在此线性范围内它们的回归方程分别是 :y =5 6 0 6× 10 3 x +1 92 9× 10 3 ,r =0 995 8;y =8 0 5 2× 10 3 x - 2 4 76× 10 3 ,r =0 9985 ;y =9 773× 10 3 x +7 6 79×10 2 ,r =0 9992。扑热息痛、扑尔敏、Vc 3种成分的含量分别为 :99 4 % ,10 0 2 % ,98 7%。RSD分别为 4 0 % ,2 4 % ,3 8% ,回收率分别为 99 4 % ,99 1% ,98 4 % ,RSD值分别为 2 8% ,3 2 % ,1 6 %。结论本方法用于Vc银翘片中扑热息痛、扑尔敏、Vc 3种成分的含量测定     

薄层色谱法检查牛奶中的三聚氰胺

目的:建立牛奶中三聚氰胺检查的薄层色谱法。方法:用固相萃取法制备供试品溶液。使用硅胶G预制板,以丙酮-氯仿-氨水(7∶0.5∶2)为展开剂,以1%对二甲氨基苯甲醛的盐酸乙醇溶液为显色剂,在紫外灯(365nm)下检视。结果:本法的专属性好,灵敏度高,检测限为0.5μg,可用于牛奶中微量三聚氰胺的检查,最低检出量为0.5 mg.kg-1。采用本法对3家公司的液态奶进行了检查,结果三聚氰胺含量均低于0.5 mg.kg-1。结论:本文建立的方法操作简便快速、灵敏度高、成本低,可用于对大量样品的筛查,特别适用于基层的推广应用。     

灰黄霉素中灰黄霉酸杂质及色泽的考查

目的:本文采用薄层色谱法考查了不同厂家灰黄霉素中灰黄霉酸杂质的存在.方法:以丙酮为溶媒,精制灰黄霉素,摸索分离条件,探讨杂质限度,考查产品色泽.结果:杂质均值为0.276%,RSD为0.168%.结论:对改进产品检验方法、提高产品质量具有一定的参考价值.     

薄层色谱扫描法检测血清中对乙酰氨基酚

目的：本研究拟采用薄层色谱扫描法建立快速测定患者血清中对乙酰氨基酚浓度的方法，为指导临床合理用药和中毒急救提供依据。方法：实验取１００μｌ血清，用蒸馏水稀释１０倍，再取１００μｌ稀释血清用乙醚提取，４０℃水浴挥干，残渣用乙醇溶解点样，展开后以λ测２４５ｎｍ，λ参３１０ｎｍ薄层扫描测定。结果：本法板间测定误差小，回收率高，线性范围宽，能准确测定患者血清浓度。结论：这一方法与文献所记载的ＨＰＬＣ和ＧＣ相比，具有简便快速、费用低和不需要做衍生化的特点，为临床急诊中毒分析和血药浓度监测提供了新的快速简便的方法     

连桂清心片的薄层色谱鉴别

目的：建立连桂清心片中甘草和黄连的薄层色谱鉴别方法,为连桂清心片质量标准提供依据。方法分别采用不同的方法处理样品,分别以甘草酸铵、盐酸小檗碱为对照品,以甘草、黄连为对照药材,在硅胶 G 薄层板上点样,以适宜的展开剂展开,取出,晾干,显色剂显色。结果在薄层色谱中能够检出连桂清心片中的甘草、黄连,连桂清心片供试品溶液色谱中,与对照品或对照药材色谱相对应位置,色谱斑点清晰,荧光斑点显示相同的颜色,分离良好且阴性对照无干扰,均能有效提供连桂清心片的鉴别特征。结论建立的两种薄层色谱鉴别方法简便,专属性强,重现性好,可用于连桂清心片的薄层定性鉴别。     

Development and validation of a high-performance thin layer chromatography method for the determination of cholesterol concentration

An accurate, sensitive, precise, reliable, and quick method for the determination of cholesterol content by high-performance thin layer chromatography is developed. In this method, aluminum-backed precoated silica gel 60 F₂₅₄ plates were used as the stationary phase and the samples were sprayed with the help of CAMAG sample applicator Linomat 5. The chromatogram was developed with the mobile phase consisting of chloroform:methanol (9.5:0.5, v/v). The samples were detected using CAMAG Scanner 4 and evaluated using the method developed on winCATS software. Densitometric analysis of cholesterol was performed in absorbance mode at 200 nm. In this solvent system, cholesterol gave a compact spot with an R_f value of 0.63 ± 0.03. The linear regression analysis of data for the calibration curve showed good linearity over a concentration range of 2–7 μg/spot with a regression value of 0.99933 and standard deviation of 1.44%. The limit of detection and limit of quantification were found to be 100 ng/spot and 500 ng/spot, respectively. Using the developed method, the concentration of cholesterol in the saponified and unsaponified egg yolk sample was determined. This method was found to be reproducible and can even be used for samples containing complex matrices.     

Gold nanoparticles grafted modified silica gel as a new stationary phase for separation and determination of steroid hormones by thin layer chromatography

A new thin layer chromatographic layer using gold nanoparticles grafted 3-triethoxysilyl propylamine modified silica gel (Au NPs-APTS modified silica gel) was developed as a stationary phase for separation and determination of two steroid hormones, namely progesterone and testosterone. Acetone–n-hexane 25:75 (v/v) was used as the mobile phase, and the results were compared with those obtained using plain (i.e., unmodified) silica gel plates. Some chromatographic parameters used for separation of the two steroids on an Au NPs-APTS modified silica gel plate as well as on a plain silica gel plate, including ΔR_F, separation factor (α), and resolution (R_S), were evaluated and compared. The reproducibility of R_F values was also determined by analysis of the two steroids in 7 consecutive days on both plates. Validity of the method was investigated, and a wide linear range of 1–200 ng per spot, and low detection limits of 0.16 ng and 0.13 ng per spot, low quantification limits of 0.51 ng and 0.40 ng per spot, and good precision (expressed as percent relative standard deviation) lower than 3.1% and 2.7% were obtained for progesterone and testosterone, respectively. As the results revealed, the proposed method is rapid and sensitive, and it is applicable to separation and determination of progesterone and testosterone in biological matrices such as urine samples.     

肝介安颗粒中黄芩和白芍的鉴别及延胡索乙素的含量测定

目的：建立肝介安颗粒剂的质量标准。方法：用薄层色谱法对处方中黄芩和白芍进行鉴别；用RP-HPLC法测定处方中延胡索乙素的含量，色谱条件：依利特ODS2柱，203．82mmol／L乙酸铵溶液-乙腈（75：25）为流动相，乙酸调pH4．4，流速0．8mL／min，检测波长280nm。结果：薄层色谱中，在对照品和生药的相应位置处，黄芩、白芍供试品分别显暗绿色和蓝紫色斑点，Rr值分别为0．65和0．40，阴性对照液没有斑点。RP-HPLC中，延胡索乙素的线性范围为10．08～120．96μg／mL，回归方程为A=17．855c＋1．8092（r=0．9996）。平均加样回收率为99．94％，RSD为1．60％（n=5）。结论：该方法简便、准确，可用于肝介安颗粒剂的质量控制。     

Development of validated high-performance thin layer chromatography for quantification of aristolochic acid in different species of the Aristolochiaceae family

This study was undertaken to isolate and quantify aristolochic acid in Aristolochia indica stem and Apama siliquosa root. Aristolochic acid is an important biomarker component present in the Aristolochiaceae family. The isolation method involved simple solvent extraction, precipitation and further purification, using recrystallization. The structure of the compound was confirmed using infrared spectroscopy, mass spectrometry and nuclear magnetic resonance. A specific and rapid high-performance thin layer chromatography (HPTLC) method was developed for analysis of aristolochic acid. The method involved separation on the silica gel 60 F₂₅₄ plates using the single solvent system of n-hexane: chloroform: methanol. The method showed good linear relationship in the range 0.4–2.0 μg/spot with r² = 0.998. The limit of detection and limit of quantification were 62.841 ng/spot and 209.47 ng/spot, respectively. The proposed validated HPTLC method was found to be an easy to use, accurate and convenient method that could be successfully used for standardization and quality assessment of herbal material as well as formulations containing different species of the Aristolochiaceae family.