Journal of Pharmaceutical Analysis

2012, 02(1): 后插1-后插3,封3-封4.

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Rapid determination of anti-estrogens by gas chromatography/mass spectrometry in urine:Method validation and application to real samples

E.Gerace, A.Salomone, G.Abbadessa, S.Racca, M.Vincenti

2012, 02(1): 1-11. doi: 10.1016/j.jpha.2011.09.011

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A fast screening protocol was developed for the simultaneous determination of nine antiestrogenic agents (aminoglutethimide,anastrozole,clomiphene,drostanolone,formestane,letrozole,mesterolone,tamoxifen,testolactone) plus five of their metabolites in human urine.After an enzymatic hydrolysis,these compounds can be extracted simultaneously from urine with a simple liquid-liquid extraction at alkaline conditions.The analytes were subsequently analyzed by fast-gas chromatography/mass spectrometry (fast-GC/MS) after derivatization.The use of a short column,high-flow carrier gas velocity and fast temperature ramping produced an efficient separation of all analytes in about 4mtin,allowing a processing rate of 10 samples/h.The present analytical method was validated according to UNI EN ISO/IEC 17025 guidelines for qualitative methods.The range of investigated parameters included the limit of detection,selectivity,linearity,repeatability,robustness and extraction efficiency.High MSsampling rate,using a benchtop quadrupole mass analyzer,resulted in accurate peak shape definition under both scan and selected ion monitoring modes,and high sensitivity in the latter mode.Therefore,the performances of the method are comparable to the ones obtainable from traditional GC/MS analysis.The method was successfully tested on real samples arising from clinical treatments of hospitalized patients and could profitably be used for clinical studies on anti-estrogenic drug administration.

Spectrofluorimetric method for determination of some angiotensin Ⅱ receptor antagonists

Salwa R.EI-Shaboury, Samiha A.Hussein, Niveen A.Mohamed, Mohamed M.EI-Sutohy

2012, 02(1): 12-18. doi: 10.1016/j.jpha.2011.10.005

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A simple,rapid,accurate and highly sensitive spectrofluorimetric method has been developed for determination of some angiotensin Ⅱ receptor antagonists (AIIRA's),namely Losartan potassium (Los-K),Irbesartan (Irb),Valsartan (Val) and Candesartan cilexetil (Cand) in pure forms as well as in their pharmaceutical dosage forms.All the variables affecting the relative fluorescence intensity (RFI) were studied and optimized.Under the optimum conditions,linear relationships with good correlation coefficients (0.9982-0.9991) were obtained over the concentra tion range from 0.006μg/mL to 1.7μg/mL.Good accuracy and precision were successfully obtained for the analysis of tablets containing each drug alone or combined with hydrochlor othiazide (HCTZ) without interferences from the co-formulated HCTZ or the additives commonly present in tablets.

Precolumn derivatization LC-MS/MS method for the determination and pharmacokinetic study of glucosamine in human plasma and urine

Min Song, Tai-Jun Hang, Cheng Wang, Lin Yang, Ai-Dong Wen

2012, 02(1): 19-28. doi: 10.1016/j.jpha.2011.08.003

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A selective precolumn derivatization liquid chromatography-tandem mass spectrometric (LC-MS/MS) method for the determination of glucosamine in human plasma and urine has been developed and validated.Glucosamine was derivatized by o-phthalaldehyde/3-mercaptopropionic acid.Chromatographic separation was performed on a Phenomenex ODS column (150 mm × 4.6mm,5μm) using linear gradient elution by a mobile phase consisting of methanol (A),and an aqueous solution containing 0.2% ammonium acetate and 0.1% formic acid (B) at a flow rate of 1 mL/min.Tolterodine tartrate was used as the internal standard (IS).With protein precipitation by acetonitrile and then the simple one-step derivatization,a sensitive bio-assay was achieved with the lower limit of quantitation (LLOQ) as low as 12 ng/mL for plasma.The standard addition calibration curves suitable for clinical sample analysis showed good linearity over the range of 0.012-8.27 μg/mL in plasma and 1.80-84.1 μg/mL in urine.The fully validated method has been successfully applied to a pharmacokinetic study of compound glucosamine sulfate dispersible tablets in health Chinese volunteers receiving single oral doses at 500,1000 and 1500 mg of glucosamine sulfate,as well as multiple oral doses of 500 mg t.i.d.for 7 consecutive days.

Analysis of in vivo absorption of didanosine tablets in male adult dogs by HPLC

Patricia Severino, Heloisa Silva, Eliana B.Souto, Maria Helena A.Santana, Teresa Cristina T.Dalla Costa

2012, 02(1): 29-34. doi: 10.1016/j.jpha.2011.10.006

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Didanosine is an effective antiviral drug in untreated and antiretroviral therapy-experienced patients with Human Immunodeficiency Virus (HIV).An automated system using on-line solid extraction and High performance Liquid Chromatography (HPLC) with ultraviolet (UV) detection was developed and validated for pharmacokinetic analysis of didanosiae in dog plasma.Modifications were introduced on a previous methodology for simultaneous analysis of antiretroviral drugs in human plasma.Extraction was carried out on C18 cartridges,with high extraction yield as stationary phase,whereas mobile phase consisted of a mixture of 0.02 M potassium phosphate buffer,acetonitrile (KH2PO4:acetonitrile:96∶4,v/v) and 0.5% (w/v) of heptane sulphonic acid.The pH was adjusted to 6.5 with triethylamine.All samples and standard solutions were chromatographed at 28℃.For an isocratic run,the flux was 1.0 mL/min,detection was at 250nm and injected volume was 20μL.The method was selective and linear for concentrations between 50 and 5000 ng/mL.Drug stability data ranged from 96% to 98%,and limit of quantification was 25 ng/mL.Extraction yield was up to 95%.Drug stability in dog plasma was kept frozen at -20℃ for one month after thee freeze-thaw cycles,and for 24 h after processing in the auto sampler.Assay was successfully applied to measure didanosine concentrations in plasma dogs.

Characterization of flavonoids in Millettia nitida vat.hirsutissima by HPLC/DAD/ESI-MSn

Min Ye, Wen-Zhi Yang, Ke-Di Liu, Xue Qiao, Bei-Jia Li, Jun Cheng, Jie Feng, De-An Guo, Yu-Ying Zhao

2012, 02(1): 35-42. doi: 10.1016/j.jpha.2011.09.009

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Millettia nitida var.hirsutissima is a Chinese herbal medicine used for the treatment of gynecological diseases.An HPLC/DAD/ESI-MSn method was established for the rapid separation and characterization of bioactive flavonoids in M.nitida var.hirsutissima.A total of 32 flavonoids were detected,of which 14 compounds were unambiguously characterized by comparing their retention time,UV,and MS spectra with those of the reference standards,and the others were tentatively identified based on their tandem mass spectrometry fragmentation data obtained in the negative ionization mode on line.Nineteen of these compounds characterized were reported from this plant for the first time.

Spectrophotometric method for the determination of ketoconazole based on amplification reactions

Shaligram S.Rane, P.Padmaja

2012, 02(1): 43-47. doi: 10.1016/j.jpha.2011.10.004

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This paper describes a sensitive spectrophotometric method developed for determination of Ketoconazole (KC) in tablets based on amplification reactions.Ketoconazole was oxidized with periodate,resulting in formation of KC2+ and iodate ions.After masking the excess periodate with molybdate,the iodate was treated with iodide to release iodine.The liberated iodine was transformed to ICl2ˉ species and extracted as ion-pair with rhodamine 6G into toluene for spectrophotometric measurement at 535nm.A linear calibration graph was obtained between 0.2136μg/mL and 1.7088 μg/mL of Ketoconazole with a molar absorptivity of 5 × 105 mol.L-1 cmˉ 1.The procedure was successfully applied for the determination of ketoconazole in tablet formulation.

High performance liquid chromatographic separation of thirteen drugs collected in Chinese Pharmacopoeia 2010(Ch.P2010) on cellulose ramification chiral stationary phase

Ying Zhou, Chao Ma, Yan Wang, Qi-Ming Zhang, Yi-Ying Zhang, Jie Fu, Hong Gao, Li-Xun Zhao

2012, 02(1): 48-55. doi: 10.1016/j.jpha.2011.11.007

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The enantiomers separation of thirteen drugs collected in Ch.P2010 was performed on chiral stationary phase of cellulose ramification (chiralpak OD and chiralpak OJ) by high performance liquid chromatographic (HPLC) methods,which included ibuprofen (Cl),ketoprofen (C2),nitrendipine (C3),nimodipine (C4),felodipine (C5),omeprazole (C6),praziquantel (C7),propranolol hydrochloride (C8),atenolol (C9),sulpiride (C10),clenbuterol hydrochloride (C11),verapamil hydrochloride (C12),and chlorphenamine maleate (C13).The mobile phase consisted of isopropanol and n-hexane.The detection wavelength was set at 254 nm and the flow rate was 0.7 mL/min.The enantiomers separation of these thirteen racemates on chiralpak OD column and chiralpak OJ column was studied,while the effects of proportion of organic additives,alcohol displacer and temperature on the separation were studied.And the mechanism of some of racemates was discussed.The results indicated that thirteen chiral drugs could be separated on chiral stationary phase of cellulose ramification in normal phase chromatographic system.The chromatographic retention and resolution of enantiomers could be adjusted by factors including column temperature and the concentration of alcohol displacer and organic alkaline modifier in mobile phase.It was shown that the resolution was improved with reducing concentration of alcohol displacer.When concentration of organic alkaline modifier was 0.2% (v/v),the resolution and the peak shape were fairly good.Most racemates mentioned above had better resolution at column temperature of 25 ℃.When racemates were separated,the temperature should be kept so as to obtain stable separation results.

Glassy carbon electrode modified with multi-walled carbon nanotubes sensor for the quantification of antihistamine drug pheniramine in solubilized systems

Rajeev Jain, Sanjay Sharma

2012, 02(1): 56-61. doi: 10.1016/j.jpha.2011.09.013

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A sensitive electroanalytical method for quantification of pheniramine in pharmaceutical formulation has been investigated on the basis of the enhanced electrochemical response at glassy carbon electrode modified with multi-walled carbon nanotubes in the presence of sodium lauryl sulfate.The experimental results suggest that the phcniramine in anionic surfactant solution exhibits electrocatalytic effect resulting in a marked enhancement of the peak current response.Peak current response is linearly dependent on the concentration of pheniramine in the range 200-1500 μg/mL with correlation coefficient 0.9987.The limit of detection is 58.31 μg/m L.The modified electrode shows good sensitivity and repeatability.

Determination of metabolite of nicergoline in human plasma by high-performance liquid chromatography and its application in pharmacokinetic studies

Rong Zheng, Yi-Hong Wu, De-Xi Jiang, Dan Zhang

2012, 02(1): 62-66. doi: 10.1016/j.jpha.2011.09.005

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A fast,simple and sensitive high performance liquid chromatographic (HPLC) method has been developed for determination of 10α-methoxy-6-methyl ergoline-8β-methanol (MDL,a main metabolite of nicergoline) in human plasma.One-step liquid-liquid extraction (LLE) with diethyl ether was employed as the sample preparation method.Tizanidine hydrochloride was selected as the internal standard (IS).Analysis was carried out on a Diamonsil ODS column (150 mm × 4.6 mm,5 μm) using acetonitrile-ammonium acetate (0.1 mol/L) (15/85,v/v) as mobile phase at detection wavelength of 224 nm.The calibration curves were linear over the range of 2.288-73.2 ng/mL with a lower limit of quantitation (LLOQ) of 2.288 ng/mL.The intra- and inter-day precision values were below 13% and the recoveries were from 74.47% to 83.20% at three qtality control levels.The method herein described was successfully applied in a randomized crossover bioequivalence study of two different nicergoline preparations after administration of 30 mg in 20 healthy volunteers.

Development and validation of a reversed-phase HPLC method for analysis of tetrahydrozoline hydrochloride in eye drop formulations

Fuad Al-Rimawi, Wahbeh Zareer, Salah Rabie, Mazen Quod

2012, 02(1): 67-70. doi: 10.1016/j.jpha.2011.11.001

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A simple,precise,accurate,and stability-indicating method is developed and validated for analysis of tetrahydrozoline hydrochloride in eye drop formulations.Separation was achieved on a reversed-phase C8 column (125 mm × 4.6 mm i.d.,5 μm) using a mobile phase consisting of acetonitrile/phosphate buffer of pH 3.0 (20∶80,v/v) at a flow rate of 1.0 mL/min and UV detection at 240 nm.This method is validated according to United States Pharmacopeia requirements for new methods,which include accuracy,precision,selectivity,robustness,and linearity and range.This method shows enough selectivity,accuracy,precision,and linearity and range to satisfy Federal Drug Administration/International Conference on Harmonization regulatory requirements.The current method demonstrates good linearity over the range of 0.025-0.075 mg/mL of tetrahydrozoline with r2 0.999.The average recovery of the method is 100.8% with a relative standard deviation of 0.47%.The degree of reproducibility of the results obtained as a result of small deliberate variations in the method parameters and by changing analytical operators has proven thai the method is robust and rugged.

Fingerprint analysis of placenta polypeptide injection by high performance liquid chromatography

LiHuang, Xiao-Man WU, Yu Ji, Yu Wang

2012, 02(1): 71-75. doi: 10.1016/j.jpha.2011.10.003

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Objective:To develop the representative fingerprint for the quality control of placenta polypeptide injection.Methods:The chromatographic separation was performed using a Phenomenex Gemini C18 column (250 mm × 4.6 mm,5 μm) maintained at 30 ℃.0.1% aqueous trifluoroacetic acid (Solvent A) and acetonitrile contained 0.1% TFA (Solvent B) were used as mobile phase with a gradient elution.Detection wavelength was 280 nm with the sample injection volume of 50 μL; the flow rate was 1.0 mL/min.The fingerprints of different samples were investigated by similarity analysis.Results:Nine peaks were identified as the characteristic common peaks.The similarities of the fingerprints of the 10 batches of samples were above 0.992.Conclusion:This method showed high precision and good repeatability,and provided the basis for the improvement of the quality control of placenta polypeptide iniection.

Determination of fluoroquinolones, sulfonamides,and tetracyclines multiresidues simultaneously in porcine tissue by MSPD and HPLC-DAD

Hu Yu, Hui Mu, Ying-Mei Hu

2012, 02(1): 76-81. doi: 10.1016/j.jpha.2011.09.007

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An efficient method is provided to detect simultaneously some important veterinary drugs from different classes in highly complex animal tissue matrix.This method using matrix solid-phase dispersion (MSPD) and high performance liquid chromatography (HPLC) with diode array detection (DAD) is developed to effectively determine two fluoroquinolones (enoxacin and lomefloxacin),two sulfonamides (sulfanilamide and sulfamethoxazole) and one tetracycline (tetracycline) simultaneously in porcine tissues.In the process,MSPD methodology was used to treat samples,washed by n-hexane to remove lipid,eluted the analytes with acetonitrile-dichloromethane (1∶1,v/v).Solvent acetonitrile and solvent acetic acid (0.1%) were combined in a gradient.HPLC-DAD analysis of the tissue samples was performed within 15min at a flow rate of 1.0mL/min.The results showed that a recovery at 0.1,0.5 and 1.0 μg/g fortification levels ranged from 80.6% to 99.2% with satisfactory relative standard deviations (RSDs) (below 6.1%.n=3) and the limits of quantitation (LOQ) ranged from 7 μg/kg to 34 μg/kg in porcine tissues.Utilization of the method in successfully simultaneous analysis of porcine tissue incurred with veterinary drug multiresidues is described.

2012 Vol. 2, No. 1