改良型比光谱-导数分光光度法在四元混合体系同时测定中的应用

提出了可应用于四元混合体系同时测定的比光谱-导数分光光度法,阐述了该方法的基本原理,并将其应用于氨基比林、苯巴比妥、咖啡因和非那西丁四元混合体系中各组分的同时测定.结果表明,氨基比林、苯巴比妥、咖啡因和非那西丁的回收率分别是109.3%(RSD=4.3%)、102.4%(RSD=6.6%)、108.7%(RSD=5.1%)、98.62%(RSD=3.2%).方法的准确度和精密度都可以满足四组分同时测定的要求,方法简单、快速.     

改良型比光谱-导数分光光度法在四元混合体系同时测定中的应用

提出了可应用于四元混合体系同时测定的比光谱-导数分光光度法，阐述了该方法的基本原理，并将其应用于氨基比林、苯巴比妥、咖啡因和非那西丁四元混合体系中各组分的同时测定。结果表明，氨基比林、笨巴比妥、咖啡因和非那西丁的回收率分别是109．3％（RSD=4．3％）、102．4％（RSD=6．6％）、108.7％（RSD=5．1％）、98．62％（RSD=3．2％）。方法的准确度和精密度都可以满足四组分同时测定的要求，方法简单、快速。     

BP网络光度法测定去痛片中的四组分

应用Levenberg-Marquardt优化算法的BP网络,采用紫外分光光度法测定去痛片中四组分的含量。测定低含量组分咖啡因和苯巴比妥时,结合吸光度减法技术。氨基比林、非那西丁、咖啡因和苯巴比妥的平均回收率和RSD分别为99.3%,1.2%：;100.0%,1.1%;100.3%,1.5%;100.1%,1.3%。     

统计模拟分光光度法同时测定复方茶碱片中的五组分含量

研究了测定复方茶碱片中五组分含量的统计模拟分光光度法。利用逐步回归分析法建立经验数学模型。再运用改良单纯形法进行优化，同时测定复方茶碱片中的五种组分-氨基比林、非那西丁、茶碱、可可碱和咖啡因的含量，其回收率分别为99.5%、100.2%、101.2%、100.2%和99.2%，RSD分别为1.51%、1.03%、4.44%、2.47%和3.12%。t检验结果证明，该方法与HPLC法之间无显著性差异。     

氨基比林的循环伏安测定及其电化学行为研究

在0.05 mol/L Tris-HCI(pH=8.5)的底液中,采用循环伏安法测定氨基比林,得到一良好的氧化峰,峰电位Ep=0.25 V,峰电流Ip与氨基比林的浓度在8.0×10-7～1.6×10-5mol/L范围内呈线性关系,相关系数r=0.9969,检出限为9.0×10-8mol/L.采用本法测定安痛定注射液中氨基比林的含量,回收率在95.0%～106.2%相对标准偏差(RSD)为1.68%.研究了氨基比林在玻碳电极上的电化学行为,结果表明氨基比林的电极过程具有吸附性和不可逆性.     

甲基原薯蓣皂苷含量的高效液相色谱法测定

建立了测定甲基原薯蓣皂苷(MPD)含量的高效液相色谱法.以甲醇制样,采用氨基柱(200mm×4.6mm,5μm),以乙腈-水(体积比90:10)流动相等度洗脱,流速1.2mL·min-1,柱温35℃,检测波长208nm;MPD在0.1008～1.008g·L-1范围内线性关系良好(r=0.9998,n=6);精密度实验的RSD为2.4%(n=6),重复性实验的RSD为1.6%(n=5),平均回收率为98.4%.3批MPD原料的批内平均含量均不少于92.89%(n=5),批间平均含量为93.78%(n=3).     

气相色谱法用于樟脑酚液的定量研究

建立了樟脑酚液中樟脑、苯酚的气相色谱定量法。樟脑的平均回收率为99.89％,RSD=0.71％(n=6);苯酚的平均回收率为100.1％.RSD=0.61％(n=6)。     

GC法同时测定酚氨咖敏片中4种组分

建立了同时测定酚氨咖敏片中对乙酰氨基酚、氨基比林、咖啡因和马来酸氯苯那敏4组分含量的毛细管气相色谱法。采用SE-30大口径毛细管色谱柱(30 m×0.53 mm,1.0μm),柱温190℃,汽化室温度220℃,检测器为FID,检测温度250℃,载气为高纯N2,分流比为1∶6,内标为盐酸麻黄碱,以无水乙醇为溶剂,样品无需衍生化处理,直接进样测定。样品中各组分完全分离,辅料无干扰,对乙酰氨基酚、氨基比林、咖啡因和马来酸氯苯那敏分别在20~2000μg/mL、15~1500μg/mL、10~500μg/mL和20~100μg/mL范围内线性关系良好(r0.999),各组分的平均回收率在99.6%~101.2%范围内,RSD2%。     

回归正交设计分光光度法测定克感敏片各组分含量

本文提出了克感敏片中氨基比林、非那西丁、咖啡因和扑尔敏四组分回归正交设计分光光度法同时测定的新方法，比ＡＫＣ法和ＣＰＡ法更简便、快速、准确。     

甘青青兰和夏至草中齐墩果酸含量的测定

运用反相高效液相色谱法测定青海产甘青青兰和夏至草中齐墩果酸的含量,为这两种药材的综合有效利用和质量检测提供依据。实验以V(甲醇)∶V(0.2%H3PO4)=86∶14为流动相,在215 nm波长条件下可以检测到:甘青青兰中齐墩果酸含量为0.32%,平均回收率为98.6%,RSD为1.5%(n=5);夏至草中齐墩果酸含量为0.053%,平均回收率为99.0%,RSD为1.7%(n=5)。     

微乳液毛细管电动色谱快速分析解热镇痛药中的有效成分

建立了微乳液毛细管电动色谱快速测定解热镇痛药中非那西丁、氨基比林和咖啡因的新方法。采用由乙酸乙酯-十二烷基硫酸钠(SDS)-正丁醇-硼砂缓冲液组成的微乳液体系,以氯霉素为内标,3种有效成分在2.5 min内完成分离,峰面积相对标准偏差(RSD)在1.2%～1.6%之间,回收率在95.6%～104.0%之间。实验考察了缓冲溶液的浓度、pH值、SDS浓度以及助表面活性剂的种类、含量对分离测定的影响。该法可用于实际样品分析。     

Quantitative Auswertung von Dünnschicht-Chromatogrammen: On line-Kopplung mit programmierbaren elektronischen Tischrechnern

A TLC method for the determination of phenacetin and caffeine in pharmaceutical preparations using a densitometer in line with an integrator and electronic desk calculator is described. The calibration curves of each compound were prepared where the higher and lower tolerance concentration levels were defined. The accuracy of the method is 1.51% (phenacetin) and 2.56% (caffeine) for two experiments carried out on each plate; 1.50% (phenacetin) and 2.64% (caffeine) for four experiments for each plate (relative standard deviation, n=18 and n=36, respectively).     

毛细管气相色谱法测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量

 用５％Ｐｈ－Ｍｅ－Ｓｉｌｉｃｏｎｅ毛细管色谱柱，ＦＩＤ，二阶程序升温，以正十六烷作为内标物测定速效伤风胶囊中对乙酰氨基酚、咖啡因、马来酸氯苯那敏的含量。浓度线性范围：对乙酰氨基酚４～２０ｇ／Ｌ，咖啡因０．０８４～０．４２ｇ／Ｌ，马来酸氯苯那敏０．１５～０．７５ｇ／Ｌ。平均回收率（ｎ＝５）：对乙酰氨基酚９９．６２％（ＲＳＤ＝０．４４％）咖啡因９６．４６％（ＲＳＤ＝１．３２％），马来酸氯苯那敏９８．５５％（ＲＳＤ＝０．６５％）。     

多波长线性回归紫外分光光度法同时测定复方阿斯匹林片中的三组分

用改进的多波长线性回归分光光度法同时测定了复方阿期匹林片中三组分的含量,模拟样品中阿斯匹林、非那西丁、咖啡因的平均回收率分别为１００．３１％、９９．８７％、１００．７７％,相对标准偏差分别为０．３５％、０．２５％、１．３７％（ｎ＝１０）。对四个批号实际样品的测定结果与标准方法一致,适物复方阿斯匹林片的常规分析。     

反相高效液相色谱-二极管阵列检测同时测定去痛片中4组分的含量

建立了一种同时测定去痛片中 4组分的含量的反相高效液相色谱法。采用YWGC1 8柱 ,以甲醇 磷酸二氢钠 (35∶6 5 )为流动相 ,流速为 1.0mL min ,用二极管阵列检测器检测 ,检测波长为 2 14nm。该方法简便快捷 ,线性范围广 ,结果准确可靠 ,用于实际样品的测定 ,结果满意。     

New method for caffeine quantification by planar chromatography coupled with electropray ionization mass spectrometry using stable isotope dilution analysis

A new high-performance thin-layer chromatography/electrospray ionization mass spectrometry (HPTLC/ESI-MS) method for the quantification of caffeine in pharmaceutical and energy drink samples was developed using stable isotope dilution analysis (SIDA). After sample preparation, samples and caffeine standard were applied on silica gel 60 F254 HPTLC plates and over-spotted with caffeine-d3 used for correction of the plunger positioning. After chromatography, densitometric detection was performed by UV absorption at 274 nm. The bands were then eluted by means of a plunger-based extractor into the ESI interface of a single-quadrupole mass spectrometer. For quantification by MS the [M+H]+ ions of caffeine and caffeine-d3 were recorded in the positive ion single ion monitoring (SIM) mode at m/z 195 and 198, respectively. The calibration showed a linear regression with a determination coefficient (R2) of 0.9998. The repeatability (RSD, n=6) in matrix was相似文献   

Automated interface for hyphenation of planar chromatography with mass spectrometry

A fully automated interface to couple high-performance thin-layer chromatography (HPTLC) with mass spectrometry (MS) is described. This universal hands-free interface connects intact normal-phase plates to any liquid chromatography/mass spectrometry (LC/MS) system without any adjustments or modifications to the mass spectrometer. The interface extracts the complete substance band with its depth profile and thus allows detections in the pg/band range. The high performance of the automated interface was evaluated through caffeine quantification in real samples, viz., energy drinks and pharmaceutical tablets, without internal standard. Following chromatographic separation on silica gel 60 F(254) HPTLC plates, caffeine bands were eluted from the plate by means of the automated interface to the electrospray ionization (ESI) source of a triple-quadrupole mass spectrometer. Since in full scan mode only the protonated molecule [M+H](+) was observed, caffeine quantification was performed using the selected-ion monitoring (SIM) mode at m/z 195. The validation showed highly reliable results for the linear range (R(2) = 0.9973), repeatability (RSD = 5.6%, n = 6) and intermediate precision (RSD = 1.5%, n = 3). Regarding accuracy the results obtained by HPTLC/MS were not statistically different (F-test, t-test) from those obtained by validated HPTLC/UV methods. Hence, this interface proved to be one of the most reliable and universal interfaces for HPTLC/MS.     

Analysis of Analgesic Tablets by Quantitative High-Performance Reversed Phase TLC

Abstract

Aspirin, phenacetin, and caffeine in two commercial analgesic tablets were determined by scanning of fluorescence-quenched zones after separation on high performance TLC plates. Assays for the components ranged from 100 to 88% of label values, and agreement between duplicate samples was better than 5%. Use of phenacetin as an internal standard for determination of aspirin and caffeine was not advantageous. The analysis serves well as an introduction to quantitative TLC in undergraduate laboratory courses.     

三重-比导数分光光度法及其应用研究

提出了可以应用于三元混合物同时测定的三重 比导数分光光度法,阐述了三重 比导数分光光度法的基本原理,研究了三重 比导数分光光度法在三元复方制剂增效联磺片中磺胺甲口恶唑(SMZ)、磺胺嘧啶(SD)、甲氧苄啶(TMP)的同时测定。试验结果表明,增效联磺片中SMZ、SD、TMP的回收率分别为102 1%(RSD=2.7%,n=20)、100.5%(RSD=1.8%,n=20)、101.2%(RSD=4 3%,n=20)。