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1.
Summary Lopinavir is a new specific and potent HIV-1 protease inhibitor. A rapid high-performance liquid chromatographic method using
UV detection, has been developed and validated for the analysis of lopinavir in plasma. This involved a single liquid-solid
extraction on an OASIS? HLB column in the presence of an internal standard. Separation was achieved on a Xterra?, C8 (150×3.9 mm I.D.) column with a mobile phase consisting of acetonitrile and water (41∶59, v/v). The detection wavelength
was 210 nm. The assay was linear from 0.187 to 10.0 μg.mL−1 and the limit of quantification was 0.187 μg.mL−1. Mean recovery was ranged from 90.7% to 97.8% for lopinavir and 97.1% for the internal standard. Day to day precision and
accuracy were less than 9.6% and 7.3% respectively. This rapid and simple method can readily be used for drug monitoring of
lopinavir, in HIV-1 infected patients. 相似文献
2.
Summary A reliable and sensitive high-performance liquid chromatographic method for the determination of the recent antidepressant
citalopram and two metabolites in human plasma has been developed. Fluorescence detection at 300 nm was used, exciting at
238 nm. Separation was obtained using a reversed-phase column (C18, 250 × 3.0 mm i.d., 5 μm) and a mobile phase. 40% acetonitrile:
60% aqueous tetramethylammonium perchlorate (pH 1.9). Calibration curves were linear over a working range: 5–300 ng mL−1 for citalopram, 2.5–150.0 ng mL−1 for desmethylcitalopram and 2.5–50.0 ng mL−1 for didesmethylcitalopram. The limits of quantitation (LOQ) were 1.5 ng mL−1 for citalopram and desmethylcitalopram and 2.0 ng mL−1 for didesmethylcitalopram. Precision data, as well as accuracy, were satisfactory and no interference from different psychotropic
drugs was found. The method was therefore suitable for therapeutic drug monitoring of citalopram and its active metabolites
in plasma of depressed patients. 相似文献
3.
Summary Stability indicating high performance liquid chromatography methods have been developed for the assay of meropenem in combination
with either dopamine (A), aminophylline (B), metoclopramide (C) or ranitidine (D) in intravenous fluid mixtures. Separations
B, C and D were performed on a polar endcapped ODS column (150×2 mm) with aqueous, pH 3.0—acetonitrile (89∶11, 88∶12, and
92∶8) eluent and detection at 270, 290, 317 nm respectively. Meropenem was linear over the concentration ranges 126.88–507.50,
131.25–525, and 131.25–525 gmg mL−1. Aminophylline, metoclopramide and ranitidine were linear over the concentration ranges 13–52, 37.5–150, and 25–100 μg mL−1. Separation A was performed on a conventional ODS column (150×2.1 mm) with aqueous, pH 3.0—acetonitrile (85∶15) eluent and
detection at 280 nm. Meropenem and dopamine were linear in the 61.25–245 and 10–40 μg mL−1 ranges, respectively. Accuracy and precision for all methods were 0.20–3.30% and 0.10–1.58%, respectively. Accelerated stability
studies have been carried out on each drug by exposure to acid, base, H2O2, and heat for different time periods. 相似文献
4.
A sensitive, simple, and accurate reversed-phase column liquid chromatographic (RP-LC) method with daidzein as an internal standard and UV detection at 348 nm has been developed for determination of linarin in beagle dog plasma. Plasma protein was precipitated by addition of acetonitrile and the remaining solution was evaporated to dryness. The resulting residue was then reconstituted in methanol and injected on to a 250 mm × 4.6 mm i.d., 5 μm particle, ODS analytical column. The mobile phase was a gradient prepared from acetonitrile and an aqueous solution (0.4%) of phosphoric acid; the flow rate was 1.0 mL min−1. Response was a linear function of concentration over the range 3.4–1,373.3 ng mL−1; the correlation coefficient (R
2) was 0.993. Mean recovery was 74.2%. Within-day and between-day precision were better than 8.8% relative standard deviation (RSD). The limit of quantification was 3.4 ng mL−1. This RP-LC method was used successfully in pharmacokinetic studies of linarin in beagle plasma after administration of Yejuhua injection. 相似文献
5.
Summary A rapid and accurate HPLC method is described for the simultaneous determination of acetaminophen, dextromethorphen hydrobromide
and pseudoephedrine hydrochloride in a new cold formulation. Chromatographic separation of the three pharmaceuticals was performed
on a Hypersil CN column (150×5.0 mm, 5 μm) with a mobile phase mixture of an ion-pairing solution, methanol and acetonitrile
(25:57:18, v/v), at a flow rate of 1.0 mL min−1, with detection at 220 nm. Separation was complete in less than 10 min. The method was validated for linearity, accuracy,
precision, limit of quantitation and robustness. Linearity, accuracy, and precision were found to be acceptable over the ranges
of 2.06∼20.6 μg·mL−1 for acetaminophen, 0.202∼2.02 mg·mL−1 for pseudoephedrine hydrochloride and 0.042∼1.06 mg·mL−1 for dextromethorphen hydrobromide. 相似文献
6.
B. Venkateswara Reddy K. V. N. Suresh Reddy J. Sreeramulu G. V. Kanumula 《Chromatographia》2007,66(1-2):111-114
A rapid, specific reversed phase HPLC method has been developed for simultaneous determination of olanzapine and fluoxetine
in their formulations. Chromatographic separation of these two pharmaceuticals was carried out on an Inertsil C18 reversed phase column (150 mm × 4.6 mm, 5 μm) with a 40:30:30 (v/v/v) mixture of 9.5 mM sodium dihydrogen phosphate (pH adjusted to 6.8 ± 0.1 with triethylamine), acetonitrile and methanol as
mobile phase. The flow rate 1.2 mL min−1 and the analytes are monitored at 225 nm. Paroxetine was used as internal standard. The assay results were linear from 25
to 75 μg mL−1 for olanzapine (r
2 ≥ 0.995) and 100–300 μg mL−1 for fluoxetine (r
2 ≥ 0.995), showed intra- and inter-day precision less than 1.0%, and accuracy of 97.7–99.1% and 97.9–99.0%. LOQ was 0.005
and 0.001 μg mL−1 for olanzapine and fluoxetine, respectively. Separation was complete in less than 10 min. Validation of the method showed
it to be robust, precise, accurate and linear over the range of analysis. 相似文献
7.
A simple reversed-phase high-performance liquid chromatographic (HPLC) method has been developed for the simultaneous determination
of the antiepileptic drugs (AEDs) zonisamide (ZNS), primidone (PRI), lamotrigine (LTG), phenobarbital (PB), phenytoin (PHT),
oxcarbazepine (OXC), and carbamazepine (CBZ) and two of their active metabolites, monohydroxycarbamazepine (MHD) and carbamazepine
10,11-epoxide (CBZE) in human plasma. Plasma (100 μL) was pretreated by deproteinization with 300 μL methanol containing 20 μg mL−1 propranolol hydrochloride as internal standard. HPLC was performed on a C8 column (4.6 mm × 250 mm; particle size 5 μm) with methanol–acetonitrile–0.1% trifluoroacetic acid, 235:120:645 (v/v), as mobile phase at a flow rate of 1.5 mL min−1. ZNS, OXC, and CBZ were monitored by UV detection at 235 nm, and PRI, LTG, MHD, PB, PHT, and CBZE by UV detection at 215 nm.
Relationships between response and concentration were linear over the concentration ranges 1–80 μg mL−1 for ZNS, 5–50 μg mL−1 for PRI, 1–25 μg mL−1 for LTG, 1–50 μg mL−1 for MHD, 5–100 μg mL−1 for PB, 1–10 μg mL−1 for CBZE, 0.5–25 μg mL−1 for OXC, 1–50 μg mL−1 for PHT, and 1–25 μg mL−1 for CBZ. Intra-day and inter-day reproducibility were adequate (coefficients of variation were ≤11.6%) and absolute recovery
ranged from 95.2 ± 6.13 to 107.7 ± 7.76% for all the analytes; for the IS recovery was 98.69 ± 1.12%. The method was proved
to be accurate, reproducible, convenient, and suitable for therapeutic monitoring of the nine analytes. 相似文献
8.
A. M. Qandil B. M. Tashtoush B. M. Al-Taani S. M. Al-Nabulsi F. Al-Zogoul 《Chromatographia》2008,67(3-4):287-291
A simple, rapid and selective RP-HPLC method was developed and validated for the determination of ketorolac and five piperazinylalkyl
ester prodrugs. A binary isocratic mobile phase composed of a mixture of 65:35 (v/v) 0.02 M phosphate buffer (pH 5.4) and acetonitrile was used on a C18 column (125 × 4 mm, 5 μm). The injection volume was 25 μL and the detection wavelength was 314 nm and the flow rate was 1.5 mL min−1. The method exhibited excellent linearity with R
2 of no less than 0.999 and intra-assay and inter-assay precision that were less than the maximum amount allowed according
to Horwitz equation. The accuracy was found to be within the allowed ±15%. The limits of detection for the analytes were between
0.060 and 0.220 μg mL−1 and the limits of quantification were between 0.183 and 0.667 μg mL−1. This method was used successfully for the study of the solubility, stability and partition coefficients of piperazinylalkyl
ester prodrugs of ketorolac. 相似文献
9.
A simple, rapid, and precise reversed-phase high-performance liquid chromatographic method has been developed for simultaneous determination of losartan potassium, ramipril, and hydrochlorothiazide. The three drugs were separated on a 150 mm × 4.6 mm i.d., 5 μm particle, Cosmosil C18 column. The mobile phase was 0.025 m sodium perchlorate–acetonitrile, 62:38 (v/v), containing 0.1% heptanesulphonic acid, pH adjusted to 2.85 with orthophosphoric acid, at a flow rate of 1.0 mL min−1. UV detection was performed at 215 nm. The method was validated for linearity, accuracy, precision, and limit of quantitation. Linearity, accuracy, and precision were acceptable in the ranges 35–65 μg mL−1 for losartan, 1.75–3.25 μg mL−1 for ramipril, and 8.75–16.25 μg mL−1 for hydrochlorothiazide. 相似文献
10.
Summary A rapid and simple liquid-chromatographic method has been developed for on-line quantification of amphetamine in biological
fluids. Untreated samples (20 μL) are injected directly into the chromatographic system and purified on a 20 mm×2.1 mm i.d.
pre-column packed with 30 μm Hypersil C18 stationary phase. After clean-up the analyte is transferred to the analytical column (125 mm×4 mm i.d., 5 μm LiChrospher
100 RP18) for derivatization and separation using a mixture of acetonitrile and the derivatization reagent (o-phthaldialdehyde andN-acetyl-L-cysteine) as the mobile phase. The experimental conditions for on-line derivatization and resolution of the amphetamine
have been optimized, and the results have been compared with those obtained by derivatizing the analyte in pre-column mode.
The method described has been applied to the determination of amphetamine in plasma and urine. Good linearity and reproducibility
were obtained in the 0.1–10.0 μg mL−1 concentration range, and limits of detection were 25 ng mL−1 and 10 ng mL−1 with UV and fluorescence detection, respectively. The procedure described is very simple and rapid, because no off-line manipulation
of the sample is required; the total analysis time is approximately 8 min. 相似文献
11.
A simple, sensitive and accurate spectrophotometric method for the determination of sulphonamides (sulphamethoxazole (SMZ),
sulphaguanidine (SGD), sulphaquinoxaline sodium (SQX), sulphametrole (SMR), and sulphadimidine sodium (SDD)) has been developed.
The charge-transfer reactions between sulphonamides as n-electron donors and 7,7,8,8-tetracyanoquinodimethane (TCNQ), 2,3-dichloro-5,6-dicyano-1,4-benzoquinone (DDQ), and 2,5-dichloro-3,6-dihydroxy-1,4-benzoquinone
(chloranilic acid, p-CLA) as π-acceptors resulting in highly coloured complexes were studied. Experimental conditions for these CT reactions were carefully
optimised. Beer’s law is valid over the concentration ranges from 4–280 μg mL−1, 4–260 μg mL−1, 4–200 μg mL−1, and 4–200 μg mL−1 of SMZ, SGD, SQX, and SDD using DDQ reagent, respectively. While the calibration curves are linear in the concentration ranges
from 4–180 μg mL−1, 4–80 μg mL−1, 4–60 μg mL−1, 4–180 μg mL−1, and 4–60 μg mL−1 of SMZ, SGD, SQX, SMR, and SDD, respectively, using TCNQ reagent and from 4–380 μg mL−1 and 4–300 μg mL−1 of SQX and SDD, respectively, using p-CLA reagent, respectively. Different analytical parameters, namely molar absorptivity
(ε), standard deviation, relative standard deviation, correlation coefficient, limit of detection, and limit of quantification,
were calculated. The results obtained by the proposed methods are in good agreement with those obtained by the official method
as indicated by the percent recovery values. 相似文献
12.
A highly sensitive high-performance liquid chromatographic method with fluorescence detection has been developed for determination
of vitamin B1. Vitamin B1 was converted into a fluorescent compound by treatment with hydrogen peroxide–horseradish peroxidase and the derivative was
subsequently analyzed by HPLC on a Waters Spherisorb ODS2 column (250 mm×4.6 mm ID, 5 μm) with 40:60 methanol–pH 8.5 acetate
buffer solution as mobile phase and fluorescence detection at 440 nm (with excitation at 375 nm). The calibration graph was
linear from 5.00×10−10 mol L−1 to 5.00×10−7 mol L−1 for vitamin B1 with a correlation coefficient of 0.9991 (n=9). The detection limit was 1.0×10−10 mol L−1. The method was successfully used for determination of vitamin B1 at pg mL−1 levels in microalgal fermentation media and seawater after solid-phase extraction. Recovery was from 89 to 110% and the relative
standard deviation was in the range 1.1 to 4.3%. 相似文献
13.
H. M. Lee C. K. Jeong S. J. Choi B. M. Yoon D. H. Na K. C. Lee H. S. Lee 《Chromatographia》2000,51(5-6):353-356
Summary An automated microbore, liquid chromatographic method with column-switching was developed for the determination of clomipramine
from human plasma samples. After direct injection of samples (60 μL), plasma proteins and clomipramine were separated in size-exclusion
mode using 20% acetonitrile in 20 mM phosphate buffer (pH 7.0) on Capcell Pak MF Ph-1 precolumn (10×4 mm I.D.). By valve switching,
a fraction containing clomipramine was directed to an intermediate column for subsequent main separation on a microbore C18 column (250×1.5 mm I.D.) using 50% acetonitrile in 20 mM phosphate buffer (pH 2.5) at 0.1 mL min−1. The method was advantageous for rapidity (total analysis time: 15 min), reproducibility (C.V.<4.8%), and increased sensitivity
(1 ng mL−1). The linearity of response was good (r
2≥0.999) over the concentration range 1–250 ng mL−1. 相似文献
14.
A new method was developed for the simultaneous determination of lidocaine, proline and lomefloxacin in human urine by capillary
electrophoresis-electrochemiluminescence detection with Ru(bpy)3
2+. Conditions of the separation and detection were investigated and optimized. It was proved that 20 mM phosphate buffer at
pH 6.7 could achieve the most favorable resolution, and the high sensitivity of detection was obtained by using the detection
potential at 1.15 V and 5 mM Ru(bpy)3
2+–60 mM phosphate buffer at pH 7.6 in the detection reservoir. The detection limits were 0.02 μg mL−1 for lidocaine, 0.03 μg mL−1 for proline and 0.06 μg mL−1 for lomefloxacin. Relative standard deviations of the ECL intensity and the migration time were 3.5 and 1.1% for 6 μg mL−1 lidocaine, 3.2 and 1.0% for 6 μg mL−1 proline and 3.7 and 1.2% for 6 μg mL−1 lomefloxacin, respectively. A baseline separation for lidocaine, proline and lomefloxacin was achieved within 360 s. The
developed method was successfully applied to determine the amounts of lidocaine, proline and lomefloxacin in human urine.
The recovery and RSD were in the range of 93.3–97.2 and 3.8–4.9%, respectively. 相似文献
15.
Summary Capillary electrophoresis with amperometric detection has been evaluated for the simultaneous determination of rutin and quercetin.
The cyclic voltammogram, hydrodynamic voltammogram, and the effects of pH, concentration of buffer and sodium dodecyl sulfate
(SDS), and amount of organic modifier on the separation and the detection were studied. The optimized conditions were: detection
potential 1.2V, separation at 12 kV, 5 s at 15 kV for sample injection, running electrolyte 20 mmol L−1 borate buffer, pH 8.8, containing 40 mmol L−1 SDS and 10% acetonitrile. The detection limit of the method was low, 0.001 and 0.0005 mg mL−1, for rutin and quercetin, respectively; the linear ranges were wide −0.005–0.5 and 0.005–0.4 mg mL−1, respectively. The variations in peak current and migration time for eight consecutive injections of a standard solution
containing 0.1 mg mL−1 of each compound were 4.78 and 3.63%, and 6.50 and 2.59% for rutin and quercetin, respectively. The levels of the two compounds
in traditional Chinese herbal drugs were easily determined. 相似文献
16.
Summary A simple, rapid and accurate, routine-HPLC method is described for simultaneous determination of acetaminophen, caffeine and
chlorpheniramine maleate in a new tablet formulation Chromatographic separation of the three pharmaceuticals was achieved
on a Hypersil CN column (150×5.0 mm, 5 μm) using a mobile phase comprising a mixture of acetonitrile, an ion-pair solution
and tetrahydrofuran (13:14:87, v/v,pH4.5). The flow-rate was changed from 1.0 mL min−1 (in 0≈7.5 min) to 1.8 mL min−1 (after 3.5 min). was complete in <10 min. The method was validated for system suitability, linearity, accuracy, precision,
limits of detection and quantitation, and robustness. Linearity, accuracy and precision were found to be acceptable over the
ranges 31.6≈315.8 μg mL−1 for acetaminophen, 9.5≈94.6 μg mL−1 for caffeine and 1.4≈13.8 μg mL−1 for chlorpheniramine maleate. 相似文献
17.
Summary A rapid, simple, accurate and sensitive liquid chromatographic assay with on-line solid-phase extraction is described for
determination of trovafloxacin in human serum. Samples were deproteinized with acetonitrile and injected on to an NH2 extraction column for sample clean-up. Thereafter, an on-line column-switching system was used for quantitative transfer
of the drug to a C18 analytical column. Separation was performed by ion-pair chromatography and detection was by ultraviolet absorbance at 275
nm. Recovery was 98.5%. The linear range was from 0.25 to 20μg mL−1, with a correlation coefficient of 0.999. Detection limit was 0.1 μg mL−1 from extraction of 25 μL serum. 相似文献
18.
Summary A high-performance liquid chromatographic method with amperometric detection has been developed for the determination of levels
of clozapine (CLZ) and its active metabolite N-desmethylclozapine (DMC) in human plasma. The analysis was performed on a 5
μm C8 reversed phase column (150×4.6 mm i.d.), with acetonitrile-phosphate buffer (pH 3.5), as the mobile phase. The detection
voltage was +800 mV and the cell and column temperature were 50°C. Linear responses were obtained between 2 ng mL−1 and 100 ng mL−1. Absolute recovery for both clozapine and desmethylclozapine exceeded 88% and the detection limit was 1 ng mL−1. Repeatability, intermediate precision and accuracy were satisfactory. The method, which is rapid, sensitive and selective,
has been applied to therapeutic drug monitoring in schizophrenic patients following administration of Leponex? tablets. In 21 patients in steady state at a mean daily clozapine dosage of 358 mg (ranging from 150 to 500 mg day−1), clozapine levels averaged 379 ng mL−1 (ranging from 102 to 818 ng mL−1) and DMC levels averaged 233 ng mL−1 (ranging from 70 to 540 ng mL−1). The method requires only a very small amount of plasma (100 μL), and thus it is suitable for pharmacokinetic studies, as
well as for therapeutic drug monitoring. 相似文献
19.
Neng Zhou Yi-Zeng Liang Ben-Mei Chen Ping Wang Xian Chen Feng-Ping Liu 《Chromatographia》2007,66(7-8):481-486
A rapid, simple and specific liquid chromatography-electrospray ionization mass spectrometry method has been developed and
validated for the determination of hydroxyzine hydrochloride in human plasma. Samples were separated using a Thermo Hypersil-HyPURITYC18
reversed-phase column (150 mm × 2.1 mm i.d., 5 μm). The mobile phase consisted of 50 mM ammonium acetate (pH 4.0)–methanol–acetonitrile
(45:36:19, v/v). Hydroxyzine and its internal standard were measured by electrospray ion source in positive selective ion monitoring mode.
The method was validated with a linear range of 1.56–200.0 ng mL−1 and the lowest limit of quantification was 1.56 ng mL−1 for hydroxyzine hydrochloride (r
2= 0.9991). The extraction efficiencies were about 70% and recoveries of the method were in the range of 93.5–104.4%. The intra-day
relative standard deviation (RSD) was less than 8.0% and inter-day RSD was within 7.4%. QC samples were stable when kept at
ambient temperature for 12 h at −20 °C for 30 days and after four freeze–thaw cycles. The method has been successfully applied
to the evaluation of pharmacokinetics and bioequivalence of two hydroxyzine hydrochloride formulations in 12 healthy Chinese
volunteers after an oral dose of 25 mg. 相似文献
20.
Summary A high-performance liquid chromatographic method, with 9-anthryldiazomethane as derivatizing agent, has been developed for
the simultaneous determination ofN-carbamoyl aspartate andl-dihydroorotate in serum. Sample preparation for 1 mL serum was by simple liquid-liquid extraction and then derivatization.
The compounds were separated on a Luna C18(2) column by use of a gradient prepared from acetonitrile and 10 mM sodium acetate
buffer, pH 6.0, and fluorimetric detection was performed at excitation and emission wavelengths of 365 nm and 412 nm, respectively.
The response was found to be linearly dependent on concentration between 0.8 and 60 μg mL−1 forl-dihydrooratate and between 0.9 and 90 μg mL−1 forN-carbamoyl aspartate; the mean recovery rates were 50 and 51%, respectively. The limits of detection and quantification were
0.33 μg mL−1 and 0.6 μg mL−1, respectively, forl-dihydroorotate and 0.4 μg mL−1 and 0.7 μg mL−1 forN-carbamoyl aspartate. This method can be used to assess accumulation ofN-carbamoyl aspartate andl-dihydroorotate in body fluids in situations where cellular pyrimidine de novo synthesis is impaired. 相似文献