Journal of Pharmaceutical Analysis

Identification and determination of the major constituents in traditional Chinese medicine Longdan Xiegan Pill by HPLC-DAD-ESI-MS

Hui Liu, Juan Su, Xu Liang, Xi Zhan, Ya-Jun He, Hai-Qiang Huang, Ji Ye, Wei-Dong Zhang

2011, 01(1): 1-7.

Abstract(357) PDF(2)

Abstract:
A novel and sensitive HPLC-UV method has been developed for the simultaneous determination of twelve major compounds in Longdan Xiegan Pill.The chemical profile of the twelve compounds,including geniposidic acid (1),geniposide(2),gentiopicroside(3),liquiritin(4),crocin(5),baicalin(6),wogonoside(7),baicalein(8),glycyrrhizic acid (9),wogonin (10),oroxylin A ( 11 ) and aristolochic acid A (12),was acquired using high-performance liquid chromatography-diode array detector coupled with an electrospray tandem mass spectrometer (HPLC-DAD-ESI-MS).The analysis was performed on a Dikma Platisil ODS C18 column (250 mm × 4.6 mm,5 μm ) with a gradient solvent system of acetonitrile-0.1% aqueous formic acid.The validation was carried out and the linearities ( r > 0.9996),repeatability (RSD<1.8%),intra- and inter-day precision (RSD<1.3%),and recoveries (ranging from 96.6% to 103.4% ) were acceptable.The limits of detection (LOD) of these compounds ranged from 0.29 to 4.17 ng.Aristolochic acid A,which is the toxic ingredient,was not detected in all the batches of Longdan Xiegan Pill.Furthermore,hierarchical cluster analysis was used to evaluate the variation of the herbal prescription.The proposed method is simple,effective and suitable for the quality control of this traditional Chinese medicine (TCM).

LC-MS determination and pharmacokinetic study of salidroside in rat plasma after oral administration of suspensions of traditional Chinese medicine Erzhi Wan and Fructus Ligustri lucidi

Ze-Yun Li, Qing Li, Jiang Lü, Jun-Hong Ling, Xi-Hua Yu, Xiao-Hui Chen, Kai-Shun Bi

2011, 01(1): 8-12.

Abstract(63) PDF(0)

Abstract:
A simple,rapid and sensitive liquid chromatography-mass spectrometry (LC-MS) method was developed for the determination of salidroside in rat plasma and study of its pharmacokinetics after oral administration of suspension of Erzhi Wan and Fructus Ligustri lucidi into Wistar rats.Plasma sample of 200 μL was extracted with acetic etherisopropanol (2:1) and the extraction was performed on a Kromasil C18 column (150 mm×4.6 mm,5 μm) with the mobile phase of methanol-water (41:59,v/v) within a run time of 6.0 min.The analyte was monitored with positive electrospray ionization (ESI) by selected ion monitoring (SIM) mode.The target ions were m/z 323.05 for salidroside and m/z 411.05 for internal standard (IS) geniposide.A good linear relationship was obtained over the range of 5.0-500.0 ng/mL and the lower limit of quantification was 5.0 ng/mL.The validated method was successfully applied to the pharmacokinetic study of salidroside in rat plasma after oral administration of suspension of Erzhi Wan and Fructus Ligustri lucidi.

Response surface optimization of microwave-assisted extraction for HPLC-fluorescence determination of puerarin and daidzein in Radix Puerariae thomsonii

Ying-Kun Liu, E Yan, Han-Ying Zhan, Zhi-Qi Zhang

2011, 01(1): 13-19.

Abstract(89) PDF(1)

Abstract:
Microwave-assisted extraction was optimized with response surface methodology for HPLC-fluorescence determination of puerarin and daidzein in Radix Puerariae thomsonii.The optimized extraction procedure was achieved by soaking the sample with 70% methanol (1:15,v/v) for 30 min,and then microwave irradiation for 11 min at a power of 600 W.Coupling the extraction process with HPLC-fluorescence presented good recovery,satisfactory precision,and good linear relation.Compared with a method from the Chinese Pharmacopoeia,the proposed method enables higher extraction efficiency and more accurate analytical results.It can be of potential value in quality assessment of Radix Puerariae thomsonii medicinal materials.

Quantification of six bioactive compounds in Zhenqi Fuzheng preparation by high-performance liquid chromatography coupled with diode array detector and evaporative light scattering detector

Yi-Kai Shi, Fang Cui, Fang-Di Hu, Ying-Yan Bi, Yu-Feng Ma, Shi-Lan Feng

2011, 01(1): 20-25.

Abstract(53) PDF(2)

Abstract:
A simple and accurate high-performance liquid chromatography (HPLC) coupled with diode array detector (DAD) and evaporative light scattering detector (ELSD) was established for the determination of six bioactive compounds in Zhenqi Fuzheng preparation (ZFP).The monitoring wavelengths were 254,275 and 328 nm.Under the optimum conditions,good separation was achieved,and the assay was fully validated in respect of precision,repeatability and accuracy.The proposed method was successfully applied to quantify the six ingredients in 31 batches of ZFP samples and evaluate the variation by hierarchical cluster analysis (HCA),which demonstrated significant variations on the content of these compounds in the samples from different manufacturers with different preparation procedures.The developed HPLC method can be used as a valid analytical method to evaluate the intrinsic quality of this preparation.

Preparation and evaluation of monolithic molecularly imprinted stationary phase for S-naproxen

De-Miao Chen, Qiang Fu, Wei Du, Si-Juan Sun, Ping Huang, Chun Chang

2011, 01(1): 26-31.

Abstract(64) PDF(0)

Abstract:
An S-naproxen (S-NAP) molecularly imprinted monolithic stationary phase (MIMSP) with specific recognition for S-NAP and naproxen (NAP) was prepared by in situ technique,utilizing 4-vinylpridine (4-VP) as a function monomer,ethylene glycol dimethacrylate (EDMA) as a cross-linking agent,and low-polar solvents (toluene and dodecanol) as porogenic solvents.The selectivity of the polymers for S-NAP and NAP was evaluated by high performance liquid chromatography (HPLC).The binding characteristics were tested by Scatchard analysis.Racemic NAP could be specifically separated to some extent.At the same time,NAP could be separated from ibuprofen under optimized conditions.Scatchard analysis showed that two classes of binding sites existed in the S-NAP-imprinted polymers,with their dissociation constants estimated to be 1.045 and 5.496 μM,respectively.The results demonstrate that S-NAP and NAP can be recognized specifically on the obtained MIMSP.

Simultaneous determination of captopril and hydrochlorothiazide by time-resolved chemiluminescence with artificial neural network calibration

Han-Chun Yao, Min Sun, Xiao-Feng Yang, Zhen-Zhong Zhang, Hua Li

2011, 01(1): 32-38.

Abstract(86) PDF(2)

Abstract:
The combined use of chemometrics and chemiluminescence (CL) measurements,with the aid of the stoppedflow mixing technique,developed a simple time-resolved CL method for the simultaneous determination of captopril (CPL) and hydrochlorothiazide (HCT).The stopped-flow technique in a continuous-flow system was employed in this work in order to emphasize the kinetic differences between the two analytes in cerium (Ⅳ)-rhodamine 6G CL system.After the flow was stopped,an initial rise of CL signal was observed for HCT standards,while a direct decay of CL signal was obtained for CPL standards.The mixed CL signal was monitored and recorded on the whole process of continuousflow/stopped-flow,and the obtained data were processed by the chemometric approach of artificial neural network.The relative prediction error (RPE) of CPL and HCT was 5.9% and 8.7%,respectively.The recoveries of CPL and HCT in tablets were found to fall in the range between 95% and 106%.The proposed method was successfully applied to the simultaneous determination of CPL and HCT in a compound pharmaceutical formulation.

Synthesis of a new chitosan derivative and assay of Escherichia coli adsorption

Bing-Bing Shang, Jun Sha, Yang Liu, Qin Tu, Man-Lin Li, Jin-Yi Wang

2011, 01(1): 39-45.

Abstract(79) PDF(0)

Abstract:
A new chitosan derivative is prepared using chitosan.Ethyl chlorocarbonate was first introduced to the hydroxyl group of phthaloylchitosan through a nucleophilic reaction.Hydrazine was then added to recover the amino groups of chitosan and promote cross-linking.The structure of this new chitosan derivative was characterized by Fourier transform infrared (FT-IR) and proton nuclear magnetic resonance (1H NMR) spectroscopy,and its physical properties were determined by X-ray diffraction (XRD),differential scanning calorimetry (DSC),and thermogravimetric analysis (TGA).The thermal and chemical stabilities of the new derivative were improved compared with those of native chitosan.Assay of Escherichia coli adhesion on a film based on this chitosan derivative showed good adsorption and biofilm formation.

Rapid europium-sensitized fluorescent determination of ulifloxacin, the active metabolite of prulifloxacin, in human serum and urine

Peng Dong, Na Xu, Bo Fu, Lei Wang

2011, 01(1): 46-50.

Abstract(80) PDF(0)

Abstract:
A new fluorescent method was developed based on the ulifloxacin-europium (Ⅲ)-sodium dodecylbenzene sulfonate system for the determination of ulifloxacin,the active metabolite of prulifloxacin.Sodium dodecylbenzene sulfonate formed a ternary complex with ulifloxacin-europium (Ⅲ) and significantly enhanced the characteristic fluorescence of europium (Ⅲ).The enhanced fluorescence intensity showed a good linear relationship with the concentration of ulifloxacin in the range of 5.0× 10 8 -2.0× 10-6M with a detection limit of 2.0× 10-10 M (3σ).This method is rapid and sensitive,and has been successfully applied to the determination of ulifloxacin in human urine and serum samples.

Flow injection chemiluminescence determination of loxoprofen and naproxen with the acidic permanganate-sulfite system

Li-Juan Wang, Yu-Hai Tang, Yang-Hao Liu

2011, 01(1): 51-56.

Abstract(75) PDF(0)

Abstract:
A novel flow injection chemiluminescence (CL) method for the determination of loxoprofen and naproxen was proposed based on the CL system of KMnO4 and Na2 SO3 in acid media.The CL intensity of KMnO4-Na2 SO3 was greatly enhanced in the presence of loxoprofen and naproxen.The mechanism of the CL reaction was studied by the kinetic process and UV-vis absorption and the conditions were optimized.Under optimized conditions,the CL intensity was linear with loxoprofen and naproxen concentration in the range of 7.0 × 10- 8 - 1.0 × 10 5 g/mL and 2.0 × 10 7 - 4.0 × 10 6 g/mL with the detection limit of 2.0 × 10 8g/mL and 3.0 × 10 sg/mL (S/N =3),respectively.The relative standard deviations were 2.39% and 1.37% for 5.0 × 10- 7 g/mL naproxen and 5.0 × 10 7 g/mL loxoprofen ( n =10),respectively.The proposed method was satisfactorily applied to the determination of loxoprofen and naproxen in pharmaceutical preparations.

Diterpenoid alkaloids from a Tibetan medicinal plant Aconitum richardsonianum var.pseudosessili florum and their cytotoxic activity

Yang-Qing He, Bing-Hua Yao, Zhan-Ying Ma

2011, 01(1): 57-59.

Abstract(62) PDF(1)

Abstract:
The chemical constituents from Aconitum richardsonianum var.pseudosessiliflorum were investigated.The roots of this plant were extracted three times with 90% EtOH at the room temperature.The ethanol extracts were combined and concentrated under reduced pressure to yield residue,which was suspended in water and successively partitioned with chloroform.The chloroform extraction was isolated and purified by silica gel and Sephadex LH-20 column chromatography. Six compounds were isolated and elucidated as delelatine (1), isodelpheline (2),3-acetylaconitine (3),isoatisine (4),nordhagenine A (5) and yunaconitine (6).Compounds 1 - 5 were obtained from Aconitum Brunneum for the first time.Compound (1) showed significant cytotoxic activities (IC50 =4.36 tμM) against the human tumor cell line P388.

INFORMATION

2011, 01(1): 60-80,封3.

Abstract(55) PDF(0)

Abstract:

2011 Vol. 1, No. 1