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Jin M.-M.,Hebei Medical University | Zhang W.-D.,Hebei Medical University | Xu Y.-M.,Hebei Institute for Food and Drug Control | Du Y.-F.,Hebei Medical University | And 4 more authors.
Journal of Separation Science | Year: 2017

Ultra high performance liquid chromatography coupled with mass spectrometry and combining a tissue-smashing extraction technique was developed for the simultaneous quantitative analysis of 12 compounds in the roots of Pulsatilla chinensis. Among them, compound 6 was characterized and accurately quantified in this herb for the first time. The parameters of extraction condition were simultaneously optimized with a Box–Behnken design and Derringer's function. The optimized conditions were as follows: sample quantity of 0.5 g, ethanol concentration of 70%, and extraction time of 200 s. Multiple-reaction monitoring scanning was employed for the quantification between positive and negative mode in a single run of 6 min. Full validation of the method was carried out, and the results indicated that the method was rapid, specific, and reliable. The developed method was successfully applied to quantify the 12 compounds in 33 batches of P. chinensis from different provinces. Moreover, the principal component analysis was performed to compare the P. chinensis collected from different provinces of China based on quantitative data and the results indicated that the content of compounds could be used to differentiate the origins of P. chinensis. These results demonstrated that this method is feasible and reliable for the quality control of P. chinensis. © 2017 WILEY-VCH Verlag GmbH & Co. KGaA, Weinheim


Song G.,Hebei Medical University | Song G.,Hebei Institute for Food and Drug Control | Zhou L.,CSPC Zhongqi Pharmaceutical Technology Shijiazhuang Co. | Sheng N.,Hebei Medical University | And 4 more authors.
Journal of Pharmaceutical and Biomedical Analysis | Year: 2015

A novel quantitative method using high-performance liquid chromatography coupled to electrospray ionization tandem mass spectrometry was developed for simultaneous determination of the 16 important bioactive constituents including nine coumarins, and seven flavonoids in Common cnidium fruit samples from different regions. The separation was performed on a C18 column with linear gradient elution of acetonitrile and 0.1% acetic acid at a flow rate of 1.0ml/min in 15min. Quantification of the analytes was achieved by use of a hybrid quadrupole linear ion-trap mass spectrometer. Multiple-reaction monitoring scanning was employed with switching electrospray ion source polarity between positive and negative modes in a single run. The validation results of the method indicated that the method was simple, rapid, specific, and reliable. The results demonstrated that the quantitative difference in content of 16 bioactive constituents was useful not only for chemotaxonomy of many samples from different sources but also for the standardization and differentiation of many similar samples. Simultaneous quantification of bioactive components by high performance liquid chromatography-tandem mass spectrometric method would be a well acceptable strategy to comprehensively control the quality of C. cnidium fruit. © 2015.


Song G.,Hebei Institute for Food and Drug Control | Jin M.,Hebei Medical University | Du Y.,Hebei Medical University | Cao L.,Hebei Medical University | Xu H.,Hebei Medical University
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2016

The detection of drug metabolites, particularly for minor metabolites, continues to be a challenge owing to the complexity of biological samples. Imperatorin is an active natural furocoumarin ingredient originating from many traditional Chinese herbal medicines. In the present study, the metabolites of imperatorin after oral administration were qualitatively investigated, and possible metabolic pathways of it were subsequently proposed. Bile samples were collected after oral administration and pretreated by the application of Waters Ostro. The QTOF-MS/MS data was acquired using ultra high performance liquid chromatography coupled to quadrupole time flight spectrometry (UPLC-QTOF-MS). Based on this analytical strategy, 32 metabolites (23 phase I and 9 phase II metabolites) were identified in rat bile. The results demonstrated that C5H8 could be easily eliminated from imperatorin forming the metabolite M1. It also indicated that imperatorin and M1 underwent extensive metabolic reactions including oxidation, hydrolysis, methylation, glucuronide conjugation, C2H5NO2S conjugation and C3H5NO2S conjugation. This is the first study of imperatorin metabolism in bile samples. The proposed metabolic pathways in this research will provide essential data for further pharmaceutical studies of other linear-type furocoumarins. © 2016.


PubMed | Hebei Institute for Food and Drug Control and Hebei Medical University
Type: | Journal: Journal of chromatography. B, Analytical technologies in the biomedical and life sciences | Year: 2016

The detection of drug metabolites, particularly for minor metabolites, continues to be a challenge owing to the complexity of biological samples. Imperatorin is an active natural furocoumarin ingredient originating from many traditional Chinese herbal medicines. In the present study, the metabolites of imperatorin after oral administration were qualitatively investigated, and possible metabolic pathways of it were subsequently proposed. Bile samples were collected after oral administration and pretreated by the application of Waters Ostro. The QTOF-MS/MS data was acquired using ultra high performance liquid chromatography coupled to quadrupole time flight spectrometry (UPLC-QTOF-MS). Based on this analytical strategy, 32 metabolites (23 phase I and 9 phase II metabolites) were identified in rat bile. The results demonstrated that C5H8 could be easily eliminated from imperatorin forming the metabolite M1. It also indicated that imperatorin and M1 underwent extensive metabolic reactions including oxidation, hydrolysis, methylation, glucuronide conjugation, C2H5NO2S conjugation and C3H5NO2S conjugation. This is the first study of imperatorin metabolism in bile samples. The proposed metabolic pathways in this research will provide essential data for further pharmaceutical studies of other linear-type furocoumarins.


Zhang X.-R.,Hebei Institute for Food and Drug Control | Zhang Y.-H.,Hebei Institute for Food and Drug Control | Jiang J.-G.,Hebei Institute for Food and Drug Control | Song G.-S.,Hebei Institute for Food and Drug Control | Zi Y.,Hebei Institute for Food and Drug Control
Asian Journal of Chemistry | Year: 2013

To establish a HPLC-MS/MS method for simultaneous determination of 18 effective components in chemical medicines for cold. The samples were extracted by methanol and were separated in an Altantis T3 column within 15 min with a gradient elution of acetonitrileammonium acetate (include 0.25 % glacial acetic acid), a tandem quadrupole mass spectrometer equipped with electrospray ionization source (ESI) was used in cationic, negative ion mode, multiple reaction monitoring was performed to quantify these compounds. Eighteen linear calibration curves were obtained, r = 0.9991. The precision of the method were good, RSD (n = 6) ranged from 0.23 % to 0.96 %. The method is simple, accurate and good reproducible for simultaneous determination multiple index components under the same chromatographic condition. It could be used to provide a reference for quality evaluation of chemical medicine for cold and monitor illegally added in traditional Chinese medicine for cold.


Yang Y.,Institute of Laboratory Animal Science | Xiu J.,Institute of Laboratory Animal Science | Zhang X.,Institute of Laboratory Animal Science | Zhang L.,Institute of Laboratory Animal Science | And 3 more authors.
Molecules | Year: 2012

Human enterovirus 71, a member of the Picornaviridae family, is one of the major causative agent of hand, foot and mouth disease in children less than six years old. This illness has caused mortalities in large-scale outbreaks in the Asia-Pacific region in recent years. No vaccine or antiviral therapy is available. In this study, antiviral effect of matrine against enterovirus 71 were evaluated in vitro and in vivo. Matrine could suppress the viral RNA copy number on rhabdomyosarcoma cells. Moreover, matrine treatment of mice challenged with a lethal dose of enterovirus 71 reduced the mortality and relieved clinical symptoms. The results showed that matrine may represent a potential therapeutic agent for enterovirus 71 infection. © 2012 by the authors.


Jiang J.-G.,Hebei Institute for Food and Drug Control | Zhang X.-R.,Hebei Institute for Food and Drug Control | Zhang Y.-H.,Hebei Institute for Food and Drug Control | Song G.-S.,Hebei Institute for Food and Drug Control
Yaoxue Xuebao | Year: 2013

This paper reports the establishment of a method for rapid identification 15 effective components of anti common cold medicine (paracetamol, aminophenazone, pseudoephedrine hydrochloride, methylephedrine hydrochloride, caffeine, amantadine hydrochloride, phenazone, guaifenesin, chlorphenamine maleate, dextromethorphen hydrobromide, diphenhydramine hydrochloride, promethazine hydrochloride, propyphenazone, benorilate and diclofenac sodium) with MRM by LC-MS/MS. The samples were extracted by methanol and were separated from a Altantis T3 column within 15 min with a gradient of acetonitrile-ammonium acetate (containing 0.25% glacial acetic acid), a tandem quadrupole mass spectrometer equipped with electrospray ionization source (ESI) was used in positive ion mode, and multiple reaction monitoring (MRM) was performed for qualitative analysis of these compounds. The minimum detectable quantity were 0.33-2.5 μg·kg-1 of the 15 compounds. The method is simple, accurate and with good reproducibility for rapid identification many components in the same chromatographic condition, and provides a reference for qualitative analysis illegally added chemicals in anti common cold medicine.


PubMed | Hebei Institute for Food and Drug Control
Type: Journal Article | Journal: Yao xue xue bao = Acta pharmaceutica Sinica | Year: 2013

This paper reports the establishment of a method for rapid identification 15 effective components of anti common cold medicine (paracetamol, aminophenazone, pseudoephedrine hydrochloride, methylephedrine hydrochloride, caffeine, amantadine hydrochloride, phenazone, guaifenesin, chlorphenamine maleate, dextromethorphen hydrobromide, diphenhydramine hydrochloride, promethazine hydrochloride, propyphenazone, benorilate and diclofenac sodium) with MRM by LC-MS/MS. The samples were extracted by methanol and were separated from a Altantis T3 column within 15 min with a gradient of acetonitrile-ammonium acetate (containing 0.25% glacial acetic acid), a tandem quadrupole mass spectrometer equipped with electrospray ionization source (ESI) was used in positive ion mode, and multiple reaction monitoring (MRM) was performed for qualitative analysis of these compounds. The minimum detectable quantity were 0.33-2.5 microg x kg(-1) of the 15 compounds. The method is simple, accurate and with good reproducibility for rapid identification many components in the same chromatographic condition, and provides a reference for qualitative analysis illegally added chemicals in anti common cold medicine.

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