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1.
HPLC法测定中成药制剂中10-羟基-2-癸烯酸的含量 总被引:6,自引:0,他引:6
采用SpherisorbC18柱,以甲醇∶水∶磷酸(45∶65∶0.5)为流动相,以UV210nm为检测波长,测定中成药制剂中10-羟基-2-癸烯酸(10-HDA)的含量,10-HDA浓度在0.006~0.030g/L范围内线性关系良好(r=0.9999,n=5),检测限为0.2mg/L(S/N=3∶1)。方法具有定量准确、快速及主峰和杂质分离度高等特点。 相似文献
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反相离子对色谱法测定化妆品中溴硝丙醇等11种防腐剂 总被引:5,自引:0,他引:5
采用反相离子对色谱法测定化妆品中溴硝丙醇等11种防腐剂,以ZorbaxC8为固定相,V(0.05mol/L磷酸二氢钠)∶V(甲醇)∶V(乙腈)=50∶35∶15的溶液为流动相,添加氯化十六烷三甲胺(浓度为2mmol/L),用磷酸调pH值为35,检测波长为254nm。样品用甲醇超声提取,回收率为85%~107%(n=6),相对标准偏差为22%~7.5%。 相似文献
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高效液相色谱法测定荧光增白剂OB 总被引:1,自引:0,他引:1
本文建立了高效液相色谱测定荧光增白剂OB,即2.5-双(5-叔丁基-2-苯并恶唑基)噻吩的方法。采用YWG C18色谱柱,四氢呋喃-水(67:33V/V)为流动相,流速1.0mL/min,紫外检测波长360nm,柱温40℃,分离时间少于11min。应用于工业产品的测定,结果满意。 相似文献
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5-磺酸钠间苯二甲酸二甲酯的高效液相色谱法分析 总被引:2,自引:1,他引:1
提出了用离子对反相高效液相色谱分析5-磺酸钠间苯二甲酸二甲酯的方法,色谱柱为HypersilBDSC18,5μm,250mm×4.6mm,流动相为V(甲醇)∶V(水)=60∶40(甲醇中含四丁基磷酸二氢铵10mmol/L),柱温为30℃,流速为0.8mL/min,进样体积为20μL,检测波长为220nm。用外标法进行了定量,相对标准偏差和回收率分别为0.26%和98.1%~99.6%。 相似文献
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固相萃取技术-HPLC测定复方甘草片中吗啡的含量 总被引:9,自引:0,他引:9
报道了用SEP-PAKC18小预柱固相萃取技术和反相高效液相色谱法测定复方甘草片中微量吗啡含量的方法。对固相萃取条件进行了研究,最终选择10%甲醇溶液为清洗溶液,70%甲醇溶液为洗脱溶液,基本消除了干扰组分对测定的影响,色谱图背景吸收小,基线平稳。色谱柱为μ-BondapakC18柱,流动相为0.1mol/LNaH2PO4溶液-甲醇(51),检测波长为286nm。平均回收率为(101.2±1.5)%,RSD为1.5%。 相似文献
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高效液相色谱法同时测定快安抗感冒液中5种组分的含量 总被引:3,自引:0,他引:3
采用高效液相色谱法(HPLC)同时测定快安抗感冒液中对乙酰氨基酚、咖啡因、盐酸甲基麻黄碱、马来酸氯苯那敏和愈创木酚甘油醚的含量。色谱柱为NOVA-PAKC_18柱,流动相为V(已腈):V(0.03mol/L磷酸氢二铵):V(0.004mol/L庚烷磺酸钠):V(三乙胺)=12:44:43.5:0.5,并用磷酸调节pH值至3.0;检测波长220nm,柱温35℃。在此色谱条件下,各组分均获得良好分离。平均回收率为98.0%~100.3%,相对标准偏差小于1.8%。 相似文献
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《Analytical letters》2012,45(6):965-976
Abstract Acetaminophen, phenylephrine, dextromethorphan, and chlorpheniramine are frequently associated in pharmaceutical formulations against the common cold. A new high performance liquid chromatography (HPLC) method has been developed for the simultaneous determination of these active pharmaceutical ingredients in pharmaceutical formulations. The separation and quantitation were achieved on a 25 cm underivatized silica column using a mobile phase of methanol: water (containing 6.0 g of ammonium acetate and 10 ml of triethylamine per liter, pH adjusted to 5.0 with orthophosphoric acid), 95:5%(v/v). Detection was carried out using a variable wavelength UV-vis detector at 254 nm for acetaminophen, at 220 nm for phenylephrine, and at 227 nm for dextromethorphan and chlorpheniramine. The method showed linearity for the acetaminophen, phenylephrine, dextromethorphan, and chlorpheniramine in the 162.5–650, 2.5–10, 7.5–30, and 1–4 µg/ml ranges, respectively. The intraday and interday RSDs ranged from 0.92 to 1.52%, 1.00 to 1.76%, 1.21 to 1.74% and 1.26 to 1.80% for the acetaminophen, phenylephrine, dextromethorphan, and chlorpheniramine, respectively. Compounds were eluted in a run time of less than 12 min. 相似文献
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A simple and rapid gas chromatographic (GC) method has been developed for the simultaneous determination of combinations of acetaminophen, phenylpropanolamine hydrochloride, guaifenesin, pseudoephedrine hydrochloride, caffeine, chlorpheniramine maleate, and dextromethorphan hydrobromide in cough and cold tablets and syrups. After extraction of the analyte with alkaline ethyl acetate, 2 microL extract was injected (splitting ratio of 50:1) into a gas chromatograph equipped with a CBP1-M25-025 fused silica capillary column (25 m x 0.22 mm; film thickness, 0.25 microm). The column temperature was held at 150 degrees C for 5 min, increased to 175 degrees C at 3 degrees C/min, and increased to 270 degreesC at 10 degrees C/min. The temperatures of the flame ionization detector and injector were maintained at 300 degrees C. The GC method is inexpensive, rapid, accurate, and precise, and thus it can be used for routine analysis of tablet and syrup preparations in quality control laboratories of pharmaceutical companies. 相似文献
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A convenient high performance liquid chromatographic method for the determination of methylxanthines in biological samples is described. Separation was achieved by reversed phase chromatography using a mobile phase consisting of tetrahydrofuran + methanol + 0.01M potassium dihydrogen phosphate, pH 3.5 (1:20:79, v/v/v), on a 7 microns C18 column and a C18 Lichrosorb precolumn at a flow rate of 0.8 mL/min. Levels varying from 0.25-16 mg/L could be detected by UV at 280 nm. In this range, standard curves were established for 4 methylxanthines: theobromine, paraxanthine, theophylline and caffeine in 4 media: mobile phase, serum, gastric and pancreatic juices, and were found to be linear (r greater than or equal to 0.9975). Overall characteristics of the method were determined as: percent recovery (89.54%), accuracy (greater than or equal to 99.4%) and reproducibility (greater than or equal to 95%). Retention times ranged from 4.21 +/- 0.01 (1-methyluric acid) to 10.8 +/- 0.03 min (caffeine). Animal experiments (5 and 10 mg/kg boluses) were used to determine caffeine half life in dog's blood (310 +/- 46 and 453 +/- 59 min, respectively) and its secretion into pentagastrin stimulated gastric juice (mean concentrations 2.51 and 6.04 mg/L; mean outputs 351 and 1206 micrograms/2.25 h; both statistically different at p less than 0.001 level). 相似文献
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A rapid reversed-phase high-performance liquid chromatographic (rp-HPLC) assay for the determination of baicalin in rat thalamus was developed. This was carried out on a Hypersil -C(18) column using 4-nitro-benzoic acid as the internal standard with a mobile phase of methanol-water-H(3)PO(4) (45:55:0.2, v/v/v). Detection was by UV at 277 nm. The calibration curve for baicalin was linear (r=0.9992) over the concentration range of 0.05--4.0 microg/mL and the limit of detection was 10 ng/mL. The coefficients of variation of intra- and inter-day assays were 2.64, 5.19 and 3.19% and 3.46, 6.21 and 5.58% at concentrations of 0.5, 1.0 and 3.0 microg/mL, respectively. The recoveries of baicalin from rat thalamus were 85.4+/- 5.62, 90.7+/- 2.43 and 89.1+/- 4.75% at concentrations of 0.5, 1.0 and 3.0 microg/mL, respectively. The method was applied to determine the time course of baicalin in rat thalamus, following a single dosage of intravenous administration of Scutellariae radix extract at 90 mg/kg of baicalin to male Wistar rats. 相似文献
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A simple and rapid high-performance liquid chromatographic method with UV detection is developed and validated to determine the concentration of voriconazole in rat and beagle dog plasma. After protein precipitation using acetonitrile, the supernatant solution is chromatographed on a Diamonsil C(18) column (250 x 4.6-mm i.d., 5 microm). The mobile phase used is a combination of acetonitrile-water-acetic acid (55:45:0.25, v/v/v) with a pH of 4.0. Detection is achieved by a UV detector monitored at a wavelength of 256 nm. The matrix calibration curves are obtained both in the concentration range of 0.10-50.0 microg/mL in rat and beagle dog plasma, with the lower limit of quantitation of 0.10 microg/mL. The intra- and inter-assay precisions in terms of % relative standard deviation are lower than 8.6% and 6.0% in rat and beagle dog plasma, respectively. The accuracy in terms of % relative error ranged from -0.5% to 8.0% and -0.5% to 6.0% in rat and beagle dog plasma, respectively. This validated method is successfully applied to determine the concentration of voriconazole in plasma after intravenous administration of 36 mg/kg voriconazole to rats and 10 mg/kg voriconazole to beagle dogs, respectively. 相似文献
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Gil-Agustí M Capella-Peiró E Monferrer-Pons L García-Alvarez-Coque MC Esteve-Romero J 《The Analyst》2001,126(4):457-464
The chromatographic behaviour of binary and ternary mixtures of several phenethylamines (phenylephrine, phenylpropanolamine, ephedrine, pseudoephedrine and methoxyphenamine) and antihistamines (pheniramine, carbinoxamine, doxylamine, chlorpheniramine, dexchlorpheniramine, dexbrompheniramine, diphenhydramine, tripolidine, azatadine and phenyltoloxamine), found in cough-cold pharmaceutical preparations, was studied using C8, C18 and cyano columns, micellar mobile phases of sodium dodecyl sulfate (SDS) and pentanol and UV detection. Using a C8 column and mobile phases of 0.05 mol l-1 SDS-6% v/v pentanol or 0.15 mol l-1 SDS-2% v/v pentanol at pH 7, more than 30 different phenethylamine-antihistamine combinations can be resolved in < 15 min. Intra- and inter-day repeatabilities and reproducibilities evaluated at three different drug concentrations (0.5, 5 and 25 micrograms ml-1, n = 10) were below 1.6, 2.5 and 2.4%, respectively. The drug amounts found in 18 formulations agreed with those declared by the manufacturers within the tolerance limits, and with those obtained using a mobile phase of 55% v/v methanol at pH 7. No interference was observed from other accompanying drugs such as acetylsalicylic acid, ascorbic acid, betamethasone, bromhexine, caffeine, codeine, dextromethorphan, paracetamol, prednisolone, salicylamide and tartrazine. The proposed procedure has the advantage over the conventional aqueous-organic procedure of using a small amount of organic solvent, which is highly retained in the SDS solution. The efficiencies are also greater. On the other hand, in the micellar system, the retentions of phenethylamines and antihistamines are similar, although the compounds can be easily resolved. In contrast, using the methanol-water mobile phase, the phenethylamines are weakly retained, whereas the antihistamines usually show a high retention. 相似文献
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A validated reversed-phase high-performance liquid chromatographic (RP-HPLC) method was developed for the determination of bergenin in rat plasma. Bergenin in rat plasma was extracted with methanol, which also acted as a deproteinization agent. Chromatographic separation of bergenin was performed on a C(18) column, with a mobile phase of methanol-water (22:78, v/v) at a flow-rate of 0.8 mL/min and an operating temperature of 40 degrees C, and UV detection was set at 220 nm. The calibration curve was linear over the range 0.25-50 microg/mL (r = 0.9990) in rat plasma. The limit of quantification was 0.25 microg/mL using a plasma sample of 100 microL. The extraction recoveries were 83.40 +/- 6.02, 81.49 +/- 2.40 and 72.51 +/- 2.64% at concentrations of 0.5, 5 and 50 microg/mL, respectively. The intra-day and inter-day precision and accuracy were validated by relative standard deviation (RSD%) and relative error (RE%), which were in the ranges 3.74-9.91 and -1.6-8.0%. After intravenous administration to rats at the dose of 11.25 mg/kg, the plasma concentration-time curve of bergenin was best conformed to a two-compartment open model. The main pharmacokinetic parameters indicated that bergenin exhibited a wide distribution and moderate elimination velocity in rat. 相似文献
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建立了可同时测定双酚伪麻干混悬剂中盐酸伪麻黄碱和氢溴酸右美沙芬含量的反相高效液相色谱方法。样品先经甲醇溶解,过滤,然后以Lichrospher C6H6化学键合硅胶为固定相、乙腈-水-H3PO4(体积比为50∶50∶0.1,pH 2.5,内含1 g/L十二烷基硫酸钠)为流动相进行色谱分离,在220 nm处定量测定。结果表明,氢溴酸右美沙芬、盐酸伪麻黄碱的质量浓度分别为1.03~206 mg/L和5~200 mg/L时,其峰面积与质量浓度的线性关系良好;批内(n=7)测定的平均相对标准偏差(RSD)分别为1.8%和1.0%,批间(n=5)测定的RSD分别为2.2%和1.5%;对双酚伪麻干混悬剂中氢溴酸右美沙芬、盐酸伪麻黄碱测定回收率分别为100.0%~101.8%和95.7%~98.7%。该法适用于双酚伪麻干混悬剂中氢溴酸右美沙芬和盐酸伪麻黄碱的质量控制及含量测定,方法准确,操作简便。 相似文献
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The chromatographic behaviour of some active ingredients in cough-cold pharmaceutical preparations, the antihistamine chlorpheniramine (or the dextro enantiomer dexchlorpheniramine), and the phenethylamines phenylephrine, phenylpropanolamine and pseudoephedrine, has been studied using a C(18) column, micellar mobile phases of sodium dodecyl sulphate (SDS) and pentanol, and with UV detection. All possible combinations of chlorpheniramine/phenethylamine were resolved and determined using a mobile phase of 0.15 M SDS-6% (v/v) pentanol at pH 7, with analysis time below 7 min. Repeatabilities and within laboratory precisions were evaluated at four different drug concentrations in the range 0.5-25 mug ml(-1) (n=5), resulting RSDs below 1.6%. The drug amounts found in the analysis of 14 commercialised preparations agreed with those declared by the manufacturers within the tolerance limits, and with those obtained using an aqueous 60% (v/v) methanol reference mobile phase. No interference was observed from other accompanying drugs such as acetylsalicylic acid, ascorbic acid, betamethasone, caffeine, codeine phosphate, diphenhydramine, lactose, paracetamol, and prednisolone. The studied combinations required a rather high amount of methanol in conventional RPLC to be eluted from the column. In contrast, the proposed procedure used a much lower amount of organic solvent (pentanol), which is highly retained in the SDS solution, being also less toxic than methanol. 相似文献