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Journal of Pharmaceutical Analysis. 2011 01(2): 后插1-后插3,前插1-前插2.

Applications of HPLC/MS in the analysis of traditional Chinese medicines

Miao Li, Xiao-Fang Hou, Jie Zhang, Si-Cen Wang, Qiang Fu, Lang-Chong He

Miao Li, Xiao-Fang Hou, Jie Zhang, Si-Cen Wang, Qiang Fu, Lang-Chong He In China.traditional Chinese medicines (TCMs) have been used in clinical applications for thousands of years.The successful hyphenation of high-performance liquid chromatography (HPLC) and mass spectrometry (MS) has been applied widely in TCMs and biological samples analysis.Undoubtedly.HPLC/MS technique has facilitated the understanding of the treatment mechanism of TCMs.We reviewed more than 350 published papers within the last 5 years on HPLC/MS in the analysis of TCMs.The present review focused on the applications of HPLC/MS in the component analysis,metabolites analysis,and pharmacokinetics of TCMs etc.50% of the literature is related to the component analysis of TCMs,which show that this field is the most popular type of research.In the metabolites analysis,HPLC coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry has been demonstrated to be the powerful tool for the characterization of structural features and fragmentation behavior patterns.This paper presented a brief overview of the applications of HPLC/MS in the analysis of TCMs.HPLC/MS in the fingerprint analysis is reviewed elsewhere. Journal of Pharmaceutical Analysis. 2011 01(2): 81-91.

Determination of phthalate esters in physiological saline solution by monolithic silica spin column extraction method

Lu Lu, Yuki Hashi, Zhi-Hua Wang, Yuan Ma, Jin-Ming Lin

Lu Lu, Yuki Hashi, Zhi-Hua Wang, Yuan Ma, Jin-Ming Lin Monolithic silica spin column extraction (MonoSpin-SPE) was developed as a simple,sensitive,and eco-friendly pretreatment method which combined with ultra-fast liquid chromatography-mass spectrometry (UFLC-MS) to determine the levels of six phthalate esters,dimethyl-(DMP),diethyl-(DEP),dipropyl-[DPrP],butyl-benzyl-(BBP),dicyclohexyl(DcHP),and di-n-octyl-(DOP) phthalate in physiological saline samples.Under optimized experimental conditions,the method was linear in the following ranges:0.2 - 50 μg/L for DMP,DEP,DPrP,DcHP and DOP; 5- 100,μg/L for BBP.The correlation coefficients (R2 ) were in the range of 0.9951- 0.9995 for all the analytes and the limits of detection (LODs) and limits of quantification (LOQs) were in the ranges of 0.02- 0.9 μg/L and 0.08- 2.7 μg/L,respectively.The pretreatment process showed good reproducibility with inter-day and intra-day relative standard deviations (RSDs) below 8.5% and 11.2%,respectively.This method was used to determine the levels of six phthalate esters in physiological saline samples and the recoveries ranged from 71.2% to 107.3%.DMP and DEP were found in actual physical saline samples (brand A and brand B). Journal of Pharmaceutical Analysis. 2011 01(2): 92-99.

Determination of wholesome elements and heavy metals in safflower (Carthamus tinctorius L.) from Xinjiang and Henan by ICP-MS/ICP-AES

Ling-Han Jia, Yi Liu, Yu-Zhen Li

Ling-Han Jia, Yi Liu, Yu-Zhen Li An inductively coupled plasma mass spectrometry (ICP-MS) or inductively coupled plasma atomic emission spectrometry (ICP-AES) was developed to determine 19 elements in safflower,a traditional Chinese medicinal herb from Xinjiang Autonomous Region and Henan Province of China.Totally 19 elements in safflower included heavy metals,i.e.As,Cd,Cu,Hg and Pb,and wholesome elements,i.e.AI,Ca,Co,Cr,Fe,Mg,Mn,Mo,Ni,P,Se,Sr,V and Zn.The results showed that the concentrations of heavy metals in safflower samples were both low,all of which met the national hygiene standards except for Pb in Xinjiang sample.Meanwhile,the distribution tendency of elements in the two samples was similar,which indicated that the plant might absorb given elements in a proportional way.The method can be used for the quality control of elements in safflower,and it provides a way for the determination of the contents of safflower from Xinjiang and Henan. Journal of Pharmaceutical Analysis. 2011 01(2): 100-103.

Chemiluminescence determination of melamine with LuminoI-K3Fe(CN)6 system

Xiao-Shuang Tang, Xi-Yan Shi, Yu-Hai Tang, Zhong-Jin Yue, Qi-Qi He

Xiao-Shuang Tang, Xi-Yan Shi, Yu-Hai Tang, Zhong-Jin Yue, Qi-Qi He A sensitive chemiluminescence(CL) method was developed for determining melamine in urine and plasma samples based on the fact that melamine can remarkably enhance the chemiluminescence of Luminol-K3 Fe(CN)6 system in alkaline medium.The determination conditions were optimized.Under optimum conditions,the chemiluminescence intensity had a good linear relationship with melamine in the range of 9.0 × 10 9 7.0 × 10 6 g/mL with a correlation coefficient of 0.9992.The detection limits (3σ) were 3.54 ng/mL for urine sample and 6.58 ng/mL for plasma sample.The average recoveries of melamine were 102.6% for urine sample and 95.1% for plasma sample.Melamine in samples was extracted with liquid-liquid extraction procedures and the assay results coincided very well with that determined with flow injection chemiluminescence method.The method provides a reproducible and stable approach for sensitive detection and quantification of melamine in urine and plasma samples. Journal of Pharmaceutical Analysis. 2011 01(2): 104-107.

Sensitive determination of 4-O-methylhonokiol in rabbit plasma by high performance liquid chromatography and application to its pharmacokinetic investigation

Ming-Yue Li, Yu-Hai Tang, Xia Liu, Hai-Yan Lü, Xi-Yan Shi

Ming-Yue Li, Yu-Hai Tang, Xia Liu, Hai-Yan Lü, Xi-Yan Shi A novel high performance liquid chromatographic method was developed for the determination of 4-O-methylhonokiol in rabbit plasma and was applied to its pharmacokinetic investigation.Plasma samples were treated by one-fold volume of methanol and acetonitrile to remove the interference proteins.A reverse phase column of SHIMPACK VP-ODS (150 mm× 4.6 mm,5.0 μm) was used to separate 4-O-methylhonokiol in the plasma samples.The detection limit of 4-O-methylhonokiol was 0.2 μg/L and the linear range was 0.012- 1.536 mg/L.The good extraction recoveries were obtained for the spiked samples (84.7%,89.3% and 87.7% for low,middle and high concentrations of added standards,respectively).The relative standard deviation of intra-day and inter-day precisions was in the range from 0.6% to 13.5%.The pharmacokinetic study of 4-O-methylhonokiol was made and the results from the plasmaconcentration curve of 4-O-methylhonokiol showed a two-apartment open model.This work developed a sensitive,stable and rapid HPLC method for the determination of 4-O-methylhonokiol and the developed method has been successfully applied to a pharmacokinetic study of 4-O-methylhonokiol. Journal of Pharmaceutical Analysis. 2011 01(2): 108-112.

Development of the fingerprints for the quality evaluation of Viscum coloratum by high performance liquid chromatography

Yun-Li Zhao, Rong-Hua Fan, Hong-Xia Yuan, Miao Yu, Kai-Shun Bi, Zhi-Guo Yu

Yun-Li Zhao, Rong-Hua Fan, Hong-Xia Yuan, Miao Yu, Kai-Shun Bi, Zhi-Guo Yu A high-performance liquid chromatography coupled ultraviolet (HPLC-UV) method was developed for a chemical fingerprint analysis of Viscum coloratum. Eighteen peaks were selected as the common peaks and Homoeriodictyol-7-O-β-D-apiosiyl-(1→2)-β-D-glucoside was used as a reference.The relative areas of common peaks were used for hierarchical clustering analysis and similarity calculation.Thirty-seven samples collected from different sources were classified imo five groups.The similarities of 21 batches Viscum coloratuma samples were beyond 0.90.The results obtained suggest that the chromatographic fingerprint can efficiently identify Viscum coloratum.Additionally,the fingerprints can then be used to evaluate the correlation between Viscum coloratum and hosts. Journal of Pharmaceutical Analysis. 2011 01(2): 113-118.

Evaluation preparation technology of Xiaochaihu granules using fingerprint-peak pattern matching

Yu-Qiong Wu, Yu-Qiang Gou, Jing Han, Ying-Yan Bi, Shi-Lan Feng, Fang-Di HU, Chun-Ming Wang An approach was proposed to evaluate preparation technology by means of fingerprint-peak matching technology of high performance liquid chromatography with diode array detector (HPLC-DAD).Similarity and hierarchical clustering analysis (HCA) were applied to identify the 15 batches of Xiaochaihu granules from different manufacturers and our laboratory,and peak pattern matching between the composite formulae and Radix Bupleuri Chinensis,which was one of the main ingredients of Xiaochaihu granules,was utilized to evaluate the preparation technology of Xiaochaihu granules via the indexes of the relative deviation of retention time (RT) and UV spectrum feature similarity of their corresponding peaks.Eleven matching peaks were found between Xiaochalhu granules and Radix Bupleuri Chinensis.However,the saikosaponin A and saikosaponin D,which are the important active components in Radix Bupleuri Chinensis,were not found in Xiaochaihu granules from any manufacturers.The peak areas of 11 characteristic peaks of Xiaochaihu granules samples formed a matrix of 11 × 15.The result of HCA showed that Xiaochaihu granules samples were divided into four kinds of category.Xiaochaihu granules samples from the same manufacturer were basically clustered of the same category.The results suggested that the saikosaponin A and saikosaponin D are prone to structural transformation under the condition of decoction and in the presence of the organic acidic components.These active components,existing in raw herb,might transform to a series of non-active secondary saikosaponin due to unfavourable preparation technology.So the conventional decoction-based preparation technology of Xiaochaihu granules might greatly affect its quality and therapeutic effectiveness. This study demonstrates that fingerprint-peak matching technology can not only be used for quality control of this composite formulae,but also provide some guidance for preparation technology of Xiaochaihu granules. Journal of Pharmaceutical Analysis. 2011 01(2): 119-124.

Using cell membrane chromatography and HPLC-TOF/MS method for in vivo study of active components from roots of Aconitum carmichaeli

Yan Cao, Xiao-Fei Chen, Di-Ya Lü, Xin Dong, Guo-Qing Zhang, Yi-Feng Chai

Yan Cao, Xiao-Fei Chen, Di-Ya Lü, Xin Dong, Guo-Qing Zhang, Yi-Feng Chai An offline two-dimensional system combining a rat cardiac muscle cell membrane chromatography time-of-flight mass spectrometry (CMC-TOF/MS) with a high performance liquid chromatography time-of-flight mass spectrometry (HPLC-TOF/MS) was established for investigating the parent components and metabolites in rat urine samples after administration of the roots of Aconitum carmichaeli.On the basis of the analysis of the first dimension,retention components of the mine sample were collected into 30 fractions (one fraction per minute).Then offline analysis of the second dimension was carried out.34 compounds including 24 parent alkaloids and 10 potential metabolites were identified from the dosed rat urine,and then binding affinities of different compounds on cell membranes were compared and influences of some functional groups on activity were estimated with the semi-quantification and curve fitting method.As a result,binding affinities decreased along with the process of deacylation,debenzoylation and demethylation,which may be related to the alleviation of toxicity in the procedure of herb processing or metabolism.Moreover,some minor components in rat urine (Songorine,14-benzoylneoline,Deoxyaconitine,etc.) exerted relatively strong affinity on cell membranes are worth exploring.The results delivered by the system suggest that the CMC can be applied to in vivo study. Journal of Pharmaceutical Analysis. 2011 01(2): 125-134.

Pharmacokinetic behavior of 16-dehydropregnenolone after intramuscular administration in rats

Hong-Ying Yang, Wen-Meng Zhang, Wen-Wen Yang, Ting Zhao, Li-Xin Sun

Hong-Ying Yang, Wen-Meng Zhang, Wen-Wen Yang, Ting Zhao, Li-Xin Sun The pharmacokinetics of 16-dehydropregnenolone (16-DHP),a sterols compound isolated from Solanum lyratum Thunb.,was investigated in rats following a single intramuscular administration (40 mg/kg).The concentration of 16-DHP in rat plasma was determined by a high performance liquid chromatography (HPLC) method with UV detection.Levonorgestrel was used as the internal standard (IS).The pharmacokinetic parameters of 16-DHP were derived by non-compartmental method.After a single intramuscular administration,the maximum plasma concentration (Cmax,) was (289 ±25)ng/mL,time to reach Cmax(tmax) was (0.38±0.14) h,the elimination half-life (t1/2) was (2.5±1.1)h,the area under the plasma concentration-time curve from time zero to the time of the last measurable concentration (AUC10-t)) was (544 ± 73 )ng· h/mL.The results indicated that 16-DHP was alsorbed quickly and eliminated rapidly in rats after the intramuscular injection. Journal of Pharmaceutical Analysis. 2011 01(2): 135-138.

The clinical value of enzyme-multiplied immunoassay technique monitoring the plasma concentrations of cyclosporine A after renal transplantation

Xiao-Hui Luo, Wu-Jun Xue, Pu-Xun Tian, Xiao-Ming Ding, Hang Yan, He-Li Xiang, Yang Li The feasibility and the clinical value of the enzyme-multiplied immunoassay technique (EMIT) monitoring of blood concentrations of cyclosporine A (CsA) in patients treated with CsA were investigated after kidney transplantation.The validation method was performed to the EMIT determination of CsA blood concentration,the CsA whole blood trough concentrations (Co) of patients in different time periods after renal transplantation were monitored,and combined with the clinical complications,the statistical results were analyzed and compared.EMIT was precise,accurate and stable,also with a high quality control.The mean postoperative blood concentration of CsA was as follows:<1 month,(281.4± 57.9)ng/mL; 2 - 3 months,(264.5 ± 41.2)ng/mL; 4 - 5 months,(236.4 ± 38.9)ng/mL; 6 - 12 months,(206.5 ± 32.6)ng/mL; >12 months,(185.6 ± 28.1)ng/mL.The toxic reaction rate of CsA blood concentration within the recommended therapeutic concentration was 14.1%,significantly lower than that of the none-recommended dose group (37.2%) (P<0.05); the transplantation rejection rate was 4.4%,significantly lower than that of the nonerecommended dose group (22.5%) (P<0.05).Using EMIT to monitor the blood concentration of CsA as the routine laboratory method is feasible,and is able to reduce the CsA toxicity and rejection significantly,leading to achieving the desired therapeutic effect. Journal of Pharmaceutical Analysis. 2011 01(2): 139-142.