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1.
A simple, rapid and sensitive CE-fluorescence (FL) detection method for the analysis of alendronate (ALEN), a bisphosphonate drug, has been developed. Using a buffer solution of 20 mM sodium phosphate (pH 10.0) and a voltage of 24 kV, separation of ALEN in a 55-cm length (35-cm effective length) capillary was achieved in 5 min. FL detection of ALEN was performed via pre-column derivatization with 2,3-naphthalene dicarbox-yaldehyde (NDA). Linear correlation (r=0.9981, n=6) between FL intensity and analyte concentration was obtained in the range of 7-200 ng/mL ALEN. The developed CE-FL method was applied to the analysis of ALEN in human urine and plasma samples. In order to eliminate the interfering matrix components, SPE using magnetic Fe(3) O(4) @Al(2) O(3) nanoparticles as solid sorbents was employed to clean the biological fluids before CE-FL analysis. The linear ranges of ALEN in urine and plasma were 5-100 ng/mL (r = 0.9982, n = 7) and 5-70 ng/mL (r = 0.9954, n = 7), respectively. The LOD and LOQ in both urine and plasma samples were 1.5 and 5 ng/mL ALEN, respectively. Total analysis time including sample pre-treatment and CE separation was less than 1.5 h.  相似文献   

2.
H Cai  C K Lim 《The Analyst》1998,123(11):2243-2245
High-performance liquid chromatographic (HPLC), capillary electrophoretic (CE) and direct spectrofluorimetric methods for the determination of temoporfin-poly(ethylene glycol) 2000 conjugate (m-THPC-PEG 2000) in plasma are described and compared. m-THPC-PEG 2000 in plasma was quantitatively extracted (recovery 101-107%) with CH3OH-DMSO (4 + 1 v/v). The supernatant after centrifugation was used for HPLC, CE or direct spectrofluorimetric determination. The major drawback of the HPLC method was that it gave a broad and split peak even under gradient elution conditions, resulting in difficulty in detection and quantification. This is because m-THPC-PEG 2000 consists of a group of compounds with an average molecular mass of approximately 8680 Da owing to the wide molecular mass distribution of PEG 2000 used in the synthesis of the drug. m-THPC-PEG 2000 gave a single and relatively sharp peak when separated by CE with sodium tetraborate buffer (pH 9.45) in the presence of sodium dodecyl sulfate as the running buffer. However, this method lacks the necessary sensitivity for detecting the drug in plasma extract because of the limited sample volume that can be injected. Direct spectrofluorimetry is the method of choice because of its simplicity, specificity and sensitivity. Using an excitation wavelength of 423 nm and the specific emission maximum of 657 nm, the fluorescence intensity could be sensitively measured. The calibration curve constructed by plotting fluorescence intensity against concentration was linear within the range 1.32-1056 ng ml-1. The detection limit (S/N = 3) was 1.32 ng ml-1 and the limit of quantification (S/N = 10) was 2.24 ng ml-1. The precision and reproducibility were assessed by repeated analysis (n = 24) of spiked plasma samples at 350.8 and 699.3 ng ml-1. The RSD was 4.5% and 1.6%, respectively.  相似文献   

3.
A stability indicating capillary electrophoretic method for separation and determination of cetirizine dihydrochloride and its major impurities in bulk and a tablet dosage form was developed. The electrophoretic separation was performed in an uncoated fused-silica capillary (75 cm × 50 μm i.d.) using 75 mM sodium phosphate (pH 2.8) as background electrolyte, with an applied voltage of +25 kV at 25°C and UV detection at 230 nm. Fexofenadine was used as internal standard. The proposed method was found selective for determination of the main drug and its major impurities. The regression data obtained from the calibration plots indicated linear relationship (r 2 = 0.998) over the concentration range of 40–240 μg/mL of cetirizine. Repeatability and reproducibility of the method, assessed as intra-day and inter-day variation and expressed as RSD (%), were 1.3 and 2.6, respectively. Stress tests on cetirizine under acidic, basic, oxidative and heat incubating at 80°C conditions revealed that no major compound was formed under the applied conditions and the proposed CE method is applicable for stability studies on cetirizine. Then, the method was successfully applied to the determination of cetirizine in bulk and a tablet dosage form.  相似文献   

4.
The development and validation of a reversed-phase liquid chromatographic (LC) method for the determination of cetirizine dihydrochloride in oral formulations are described. An isocratic LC analysis was performed on a reversed-phase C18 column (250 x 4.6 mm id, 5 microm particle size). The mobile phase was 1% orthophosphoric acid solution, pH 3.0-acetonitrile (60 + 40, v/v), pumped at a constant flow rate of 1.0 mL/min. Measurements were made at a wavelength of 232 nm. The calibration curves were linear over the range of 10-30 microg/mL (r2 = 0.9999). The relative standard deviation (RSD) values for intraday precision were 0.94 and 1.43% for tablets and compounded capsules, respectively. The RSD values for interday precision were 0.13 and 0.82% for tablets and compounded capsules, respectively. Recoveries ranged from 97.7 to 101.8% for tablets and from 98.4 to 102% for compounded capsules. No interferences from the excipients were observed. Because of its simplicity and accuracy, the method is suitable for routine quality-control analysis for cetirizine in tablets and compounded capsules.  相似文献   

5.
Isoniazid and cetirizine do not retain well on reversed-phase columns due to their high polarity. Silica columns, when operated under hydrophilic interaction conditions, do provide excellent retention of these compounds. We have developed simple and proof of concept analytical methods for the analysis of isoniazid and cetirizine in animal and human plasma, respectively. Both methods employed the approach of direct injection of solid-phase extraction (SPE) organic eluents onto silica columns for analysis, thus eliminating evaporation and reconstitution steps that are typically needed for reversed-phase liquid chromatographic analysis. Isoniazid was extracted from animal plasma samples using a Waters Oasis HLB 96-well plate and then eluted with acetonitrile, while cetirizine was extracted from human plasma with a Waters MCX mu-Elute plate and then eluted with acetonitrile containing 5% concentrated ammonium hydroxide. The direct injection of the SPE eluent onto the analytical column was necessary since significant loss of isoniazid was found during the evaporation and reconstitution steps. The method for isoniazid also enabled ultra-fast analysis due to the relatively low back-pressure exhibited by silica columns even under high flow conditions. Both methods show good linearity, accuracy and precision covering the range of 10-2000 ng/mL of isoniazid, and 1-1000 ng/mL of cetirizine in plasma. Substantial time savings were realized as a result of both the elimination of the evaporation and reconstitution steps and the fast chromatographic analysis.  相似文献   

6.
Sensitive enantioselective liquid chromatographic assays using tandem mass spectrometric detection were developed and validated for the determination of S-cetirizine (S-CZE) and R-cetirizine (R-CZE) in guinea pig plasma, brain tissue, and microdialysis samples. Enantioselective separation was achieved on an alpha1-acid glycoprotein column within 14 min for all methods. A cetirizine analog, ucb 20028, was used as internal standard. Cetirizine and the internal standard were detected by multiple reaction monitoring using transitions m/z 389.1 --> 200.9 and 396.1 --> 276.1, respectively. The samples were prepared using protein precipitation with acetonitrile. For guinea pig plasma, the assay was linear over the range 0.25-5000 ng/mL for both S-CZE and R-CZE, with a lower limit of quantification (LLOQ) of 0.25 ng/mL. For the brain tissue and microdialysis samples, the assays were linear over the range 2.5-250 ng/g and 0.25-50 ng/mL, respectively, and the LLOQ values were 2.5 ng/g and 0.25 ng/mL, respectively. The intra- and inter-day precision values were < or =7.1% and < or =12.6%, respectively, and the intra- and inter-day accuracy varied by less than +/-8.0% and +/-6.0% of the nominal value, respectively, for both enantiomers in all the matrices investigated.  相似文献   

7.
Nojavan S  Fakhari AR 《Electrophoresis》2011,32(6-7):764-771
In the present study, a very simple CE method for chiral separation and quantitation of zwitterionic cetirizine (CTZ), as the main metabolite of hydroxyzine (HZ), and HZ has been developed. In addition, the effect of zwitterionic property of CTZ on enantioseparation was investigated. Maltodextrin, a linear polysaccharide, as a chiral selector was used and several parameters affecting the separation such as pH of BGE, concentration of chiral selector and applied voltage were studied. The best BGE conditions for CTZ and HZ enantiomers were optimized as 75 mM sodium phosphate solution at pH of 2.0, containing 5% w/v maltodextrin. Results showed that, compared to HZ, pH of BGE was an effective parameter in enantioseparation of CTZ due to the zwitterionic property of CTZ. The linear range of the method was over 30-1200 ng/mL for all enantiomers of CTZ and HZ. The quantification and detection limits (S/N=3) of all enantiomers were 30 and 10 ng/mL, respectively. The method was used to quantitative enantioseparation of CTZ and HZ in spiked human plasma.  相似文献   

8.
A simple and sensitive HPLC method has been developed for the determination of danofloxacin (DAN) in plasma. Sample preparations were carried out by adding phosphate buffer (pH 7.4, 0.1 M), followed by extraction with trichloromethane. DAN and the internal standard, sarafloxacin (SAR), were separated on a reversed-phase column, and eluted with aqueous solution-acetonitrile (80:20 v/v). The fluorescence of the column effluent was monitored at lambda(ex) = 338 and lambda(em) = 425 nm. The retention times were 2.80 and 4. 40 min for DAN and SAR, respectively. The method was shown to be linear from 1 to 1500 ng/mL (r(2) = 0.999). The detection and quantitation limit were 1 and 5 ng/mL, respectively. Mean recovery was determined as 80% by the analysis of plasma standards containing 150, 750 and 1500 ng/mL. Inter- and intra-assay precisions were 4.0% and 2.4%, respectively.  相似文献   

9.
A sensitive enantioselective high-performance liquid chromatography (HPLC) method was developed and validated to determine S-(+)- and R-(-)-arotinolol in human plasma. Baseline resolution was achieved by using teicoplanin macrocyclic antibiotic chiral stationary phase (CSP) known as Chirobiotic T with a polar organic mobile phase consisting of methanol:glacial acetic acid:triethylamine, 100:0.1:0.1, (v/v/v) at a fl ow rate of 0.8 mL/min and UV detection set at 317 nm. Human plasma was spiked with stock solution of arotinolol enantiomers and labetalol as the internal standard. The assay involved the use of liquid-liquid extraction procedure with ethyl ether under alkaline condition for human plasma sample prior to HPLC analysis. Recoveries for S-(+)- and R-(-)-arotinolol enantiomers were in the range 93-103% at 200-1400 ng/mL level. Intra-day and inter-day precision calculated as %RSD was in the ranges 1.3-3.4 and 1.9-4.5% for both enantiomers, respectively. Intra-day and inter-day accuracies calculated as percentage error were in the ranges 1.2-3.5 and 1.5-6.2% for both enantiomers, respectively. Linear calibration curves in the concentration range 100-1500 ng/mL for each enantiomer showed a correlation coefficient (r) of 0.9998. The limit of quantitation (LOQ) and limit of detection (LOD) for each enantiomer in human plasma were 100 and 50 ng/mL (S/N = 3), respectively.  相似文献   

10.
A validated high-performance liquid chromatography (HPLC) method was developed for simultaneous determination and pharmacokinetic study of aloe emodin and chrysophanol in rats. It was performed on a reverse-phase C(18) column and a mobile phase made up of methanol and 0.2% acetic acid (83:17, v/v). The ultraviolet detection was 254 nm. 1,8-dihydroxyanthraquinone was used as the internal standard. The assay was linear over the range 28-2800 ng/mL (r(2) = 0.9993) for aloe emodin and 25.6-2560 ng/mL (r(2) = 0.9991) for chrysophanol. The average percentage recoveries of three spiked plasmas were 98.8-104.8% and 97.7-103.2% for aloe emodin and chrysophanol, respectively. Their RSD of intra-day and inter-day precision at concentrations of 56, 280 and 1400 ng/mL for aloe emodin and 51.6, 258 and 1290 ng/mL for chrysophanol were less than 3.5%. This method was applied for the first time to simultaneously determinate aloe emodin and chrysophanol in rats following oral administration of traditional Chinese medicine of Da-Cheng-Qi decoction. The pharmacokinetic parameters showed that chrysophanol was better absorbed with higher concentrations in plasma than aloe emodin did. They both eliminated slowly in male rats. The assay is suitable for identifying the plasma and tissue levels of aloe emodin and chrysophanol in preclinical investigations.  相似文献   

11.
A platform for the pharmacokinetic study of multiple constituent traditional Chinese medicine was developed and validated. An HPLC/ESI/MS method was employed for the simultaneous determination of panax notoginsenoside R1, ginsenoside Rg1, Rd, Re and Rb1 in rat plasma. After the addition of digoxin as an internal standard (IS), rat plasmas were extracted with n-butanol saturated with pure water and all analytes were separated on a reversed-phased C(18) column with a mobile phase of acetonitrile-water (0.5 mM ammonium chloride) and pumped at a flow rate of 0.2 mL/min. Analytes were determined in a single quadrupole mass spectrometer using an electrospray ionization source. HPLC/ESI/MS was performed in the selected-ion monitoring mode with the chlorinated adducts of molecular ions [M + Cl]( -) at m/z 967.75, 835.80, 981.80, 981.80, 1143.65 and 815.40 for R1, Rg1, Rd, Re, Rb1 and digoxin, respectively. The method showed excellent linearity over the concentration range 3.03-775.00 ng/mL (r(2) = 0.9994) for R1, 4.00-1025.00 ng/mL (r(2) = 0.9991, 0.9988, 0.9991) for Rg1, Rd and Re, respectively, and 2.77-710.00 ng/mL for Rb1 (r(2) = 0.9990). The low limit of quantification was 3.03, 4.00, 4.00, 4.00 and 2.77 ng/mL for R1, Rg1, Rd, Re and Rb1, respectively, with S/N > 10. The intra- and inter-day precisions were below 12.00% and the accuracy was between -2.31 and +4.43% for all analytes. The extract recoveries of analytes were from 67.47 to 94.18%. All analytes were stable in rat plasma after storage for 12 h at ambient temperature, at 4 degrees C for 12 h in the sample pool, at -20 degrees C for 4 weeks and at -20 degrees C for three thaw-freeze cycles. The HPLC/ESI/MS technique provided an excellent method for the simultaneous quantification of R1, Rg1, Rd, Re and Rb1 in rat plasma and was successfully applied to the pharmacokinetic study of a multiple-constituent traditional Chinese medicine, total panax notoginsenoside (Xuesaitong injection).  相似文献   

12.
提出一种直接进样测定大鼠血浆中舒必利浓度的高效液相色谱方法,使用限进介质色谱柱作为预柱在线去除血浆蛋白后,将舒必利通过柱切换转移到分析柱中进行分析。限进介质色谱柱为CAPCELLPAKMFSCX阳离子交换柱(20&#215;4.0mmi.d.,5μm),分析柱为Kromasil C18柱(150&#215;4.6mm i.d.,5μm),限进介质柱预分离时流动相为PH=6.88的50mmol/L磷酸盐缓冲液乙腈(100:5,V/V),切换后分析流动相为PH=6.83的50mmol/L磷酸盐缓冲液-乙腈(100:10,V/V)。流速均为1mL/min,检测波长为240nm。该方法检出限为17ng/mL,定量限为50ng/mL。舒必利在50~1400ng/mL之间线性良好(r=0.9997),高中低浓度的日内、日间相对标准偏差分别为1.5%~4.2%及2.0%~5.2%,方法回收率为98.8%~104.1%.  相似文献   

13.
A rapid and sensitive HPLC method for the simultaneous quantitation of ondansetron and tropisetron, two serotonin (5-HT) receptor antagonists frequently used in treatment and prevention of nausea and emesis, is described. The procedure involves liquid-liquid extraction of human plasma with dichloromethane coupled with reversed-phase HPLC and UV detection. The lower limits of quantification (LOQ) were 0.62 ng/mL for ondansetron and 1.25 ng/mL or tropisetron. Intra- and inter-assay coefficients of variation ranged from 1.5 to 7.5% and 5.3 to 13.7%, respectively. The sensitivity and precision were sufficient for determination of plasma concentrations after therapeutic administration of both drugs and the method can be used for the estimation of pharmacokinetic parameters.  相似文献   

14.
A high-performance liquid chromatography (HPLC) assay is described for the determination of indomethacin in porcine plasma using acetonitrile to precipitate plasma proteins and for the one-step extraction. Calibration curves (using the internal standard method) are linear (r2 > 0.98) over the concentration range of 50.0 to 3000 ng/mL in both mobile phase and plasma. Precision, expressed as the inter- and intraday coefficient of variation (n = 5), is < 7% on the same day and < 5% between days at each plasma control sample of 300, 1000, and 3000 ng/mL, respectively. System precision, calculated as the coefficient of variation (n = 5), is < 7% at 3000 ng/mL of indomethacin, and the limit of quantitation in plasma is 50 ng/mL. The absolute recovery for both indomethacin and the internal standard (mefenamic acid) from plasma is over 97% (n = 3), and the concentrations do not deviate more than -2.9% to 2.4% from their actual values. The specificity of the method is confirmed. This technique is thus reported to be both rapid and specific. The real advantage is the small sample volume required (500 microL), which allows it to be considered for the quantitation of indomethacin in plasma from paediatric patients.  相似文献   

15.
A sensitive and rapid method based on liquid chromatography/tandem mass spectrometry (LC/MS/MS) combined with rapid solid-phase extraction (SPE) has been developed and validated for the quantitative determination of enalapril and its active metabolite enalaprilat in human plasma. After addition of internal standard to human plasma, samples were extracted by 96-well SPE cartridge. The extracts were analyzed by HPLC with the detection of the analyte in the multiple reaction monitoring (MRM) mode. This method for the simultaneous determination of enalapril and enalaprilat was accurate and reproducible, with respective limits of quantitation of 0.2 and 1.0 ng/mL in plasma. The standard calibration curves for both enalapril and enalaprilat were linear (r(2) = 0.9978 and 0.9998) over the concentration ranges 0.2-200 and 1.0-100 ng/mL in human plasma, respectively. The intra- and inter-day precision over the concentration range for enalapril and enalaprilat were lower than 13.3 and 15.4% (relative standard deviation, %RSD), and accuracy was between 89.2-105.0 and 91.9-104.7%, respectively.  相似文献   

16.
This work describes two high-performance liquid chromatographic methods for the individual determination of bisoprolol and metoprolol in human plasma. Analytical methods involve two different liquid-liquid extractions of human plasma, with diethyl ether for bisoprolol and with dichloromethane for metoprolol, coupled with a similar Nucleosil C(18) reversed-phase HPLC column. Fluorimetric detection was used to identify both beta-blockers. Retention times for bisoprolol and metoprolol were 8.7 and 3.2 min, respectively. Linear regressions for the calibration curves were linear at a concentration range of 6.25-200 ng/mL. Intra- and inter-day precision coefficients of variations and accuracy bias were acceptable (within 15%) over the entire range for both drugs. Average recovery was 89% for metoprolol and 98% for bisoprolol. Once the methods had been validated, analytical error functions were established as standard deviation (SD; ng/mL) = 2.216 + 3.608 x 10(-4)C(2) (C = theoretical concentration value) and SD-(ng/mL) = 0.408 + 0.378 x 10(-1)C for bisoprolol and metoprolol, respectively. The methods developed and their associated analytical error functions will be suitable for pharmacokinetic studies and for determination of plasma concentration if posology individualization of these drugs is needed.  相似文献   

17.
建立了高效液相色谱-荧光法同时测定癌症病人尿液中黄蝶呤及异黄蝶呤的新方法。选择荧光检测波长λex=345nm,λem=420nm。以磷酸盐缓冲溶液(pH=7.5)-甲醇(体积比为98∶2)为流动相,流速1.0mL/min,黄蝶呤与异黄蝶呤含量分别在0.0013~0.945μg/mL及0.00017~0.118μg/mL范围内与色谱峰面积呈良好的线性关系,线性相关系数分别为0.9999和0.9996,检出限分别为0.5ng/mL和0.05ng/mL,加标平均回收率在86.2%~107.5%之间。方法应用于癌症病人尿样分析,取得了较好的结果。  相似文献   

18.
This paper describes highly sensitive HPLC methods for the determination of amphetamine (AP) and methamphetamine (MP) in abusers' plasma and hair samples. AP and MP were derivatized with the fluorescent reagent, DIB-Cl, to yield a highly fluorescent DIB-derivatives of AP and MP, which were then analyzed by HPLC with fluorescence detection at excitation and emission wavelengths of 325 and 430 nm, respectively. The separation was achieved on an ODS column with isocratic mobile phases composed of acetoniltrile and citrate buffer (55:45, v/v) for plasma samples and of acetonitrile-methanol-citrate buffer (45:20:37.5, v/v/v) for hair samples. The limits of detection were less than 0.87 ng/mL and 0.12 ng/mg in plasma and hair samples, respectively, for both AP and MP. The methods were then applied to the determination of MP and its metabolite AP in plasma obtained from two cases of illegally ingested MP and in one of the cases' hair received later. Case I was treated with dialysis; samples before and after dialysis were analyzed by the described method. After dialysis for 5 h, the total plasma levels of AP and MP decreased from 720 to 190 ng/mL. For case II, MP and AP levels were monitored for 3 days after digestion. Total plasma levels decreased from 57 ng/mL in the day of digestion to 11 ng/mL after 3 days. In hair samples, AP and MP could also be detected in very low concentrations.  相似文献   

19.
A high-performance liquid chromatographic (HPLC) method is described for the simultaneous determination of sophoridine and matrine in rat plasma. Sophoridine and matrine in the resulting supernatant of the plasma deproteinized with acetonitrile containing an internal standard (acetanilide) were directly determined by reversed-phase HPLC and ultraviolet detection. The result of limits of quantitation for matrine and sophoridine were 200 and 350 ng/mL in plasma, respectively, and recovery of both analytes was greater than 98%. The assay was linear from 250 to 4000 ng/mL for matrine and from 500 to 8000 ng/mL for sophoridine. Variation over the range of the standard curve was less than 15%. The method was used to determine the concentration-time profiles of matrine and sophoridine in the plasma following oral administration of Kexieling tablets, which is one of the preparations of Kudouzi at a dose equivalent to 30 and 60 mg/kg of matrine and sophoridine, respectively.  相似文献   

20.
Two novel analytical methodologies using capillary electrophoresis (CE) and high-performance liquid chromatography (HPLC) were developed and compared for the determination of benzyldimethyldodecylammonium bromide (BAB) in commercial compound chemical disinfectants. The LC analysis was performed with a Kromasil C18 (200 mm x 4.6 mm, 5 microm) column and a mobile phase of A:B = 80:20 (A: acetonitrile, B: 4 mmol/L octanesulfonic sodium--0.02 mol/L acetic sodium, adjusted with acetic acid to pH 5.2) at a flow rate of 1.0 mL/min. Detection was by ultraviolet absorption at 262 nm. The CE analysis was performed in a bare fused-silica capillary with 75 microm i.d. and total length of 46.4 cm with a buffer solution of 50% acetonitrile -50 mmol/L NaH2PO4, pH 2.24. The applied voltage was 20 kV. Detection was by ultraviolet absorption at 214 nm. Under optimized conditions, the HPLC retention time and CE migration time for BAB was 9.18 and 5.08 min, respectively. Calibration curves of peak area versus concentration gave correlation coefficients of 0.9996 for HPLC and 0.9994 for CE. The detection limits for HPLC and CE were 1.6 mg/L and 0.2 mg/L, respectively. Average recoveries at three concentration levels (50, 100, 200 mg/L for HPLC: 20, 40, 100 mg/L for CE) were 99.94 +/- 1.5, 99.64 +/- 1.3 and 99.61 +/- 0.4% for HPLC and 120.47 +/- 2.6, 102.06 +/- 8.7 and 103.05 +/- 3.0% for CE, respectively. Although both methods were shown to be suitable for the determination of BAB in commercial disinfectant compounds, CE provided analysis with less solvent purchase/disposal and better column efficiency, whereas HPLC provided superior precision.  相似文献   

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