Sichuan Provincial Institute for Food and Drug Control

Chengdu, China

Sichuan Provincial Institute for Food and Drug Control

Chengdu, China
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Du G.,University of Macau | Zhao H.Y.,University of Macau | Zhang Q.W.,University of Macau | Li G.H.,University of Macau | And 4 more authors.
Journal of Chromatography A | Year: 2010

A microwave-assisted extraction (MAE) and ultra high performance liquid chromatography coupled with diode array detection and time-of-flight mass spectrometry (UHPLC-DAD-TOF-MS) method was developed for simultaneous determination of 14 phenolic compounds in the root of Pueraria lobata (Wild.) Ohwi and Pueraria thomsonii Benth. Operational conditions of MAE were optimized by central composite design (CCD). The optimized result was 65% ethanol as extraction solvent, 17 mL of extraction volume, 100 °C of extraction temperature and 2 min of hold time. A Zorbax SB C18 (50 mm × 4.6 mm I.D., 1.8 μm) and gradient elution were used during the analysis. The chromatographic peaks of 14 investigated compounds in samples were successfully identified by comparing their retention time, UV spectra and TOF mass data with the reference substances. All calibration curves showed good linearity (r > 0.9997) within the test ranges. The intra-day and inter-day variations were less than 1.77% and 2.88%, respectively. The developed method was successfully applied to determine the investigated compounds in 10 samples of Radix Puerariae Lobatae and Radix Puerariae Thomsonii, respectively. The result indicated that MAE and UHPLC-DAD-TOF-MS system might provide a rapid method for the quality control of Radix Puerariae.


Lv G.,Chengdu University of Traditional Chinese Medicine | Lv G.,Hong Kong Baptist University | Cheng S.,Sichuan Provincial Institute for Food and Drug Control | Chan K.,Hong Kong Baptist University | And 2 more authors.
Zhongguo Zhongyao Zazhi | Year: 2010

Ferulic acid (FA) is one of the main bioactive compounds in Chuanxiong (CX), the dried rhizome of Ligusticum chuanxiong, but its amount in this herb is difficult to determine accurately. An accurate quantificational method was developed to investigate on the available amount of FA (free FA and total FA). Herbal samples were extracted in methanol-formic acid (95:5) and methanol-0.24 mol·L-1 sodium hydrogen carbonate in water (95:5), respectively and then quantitatively analyzed by HPLC method. Thirty three CX samples were quantified on free and total FA. Total FA was found more abundant than free FA with an average ratio of 2.38 (n=32) in the range of 1.03-4.98 in 32 CX herbs, and a highest ratio of 19.6 was estimated in a rhizome seedling. Results showed that total FA content would be a better marker for the quality assessment of CX herbs. Fifteen CX typical samples were collected from the trueborn cultivating areas in Sichuan province of China. The amount of total FA in these herbs was estimated to be 1.42 mg·g-1 (n=15). The proposed limit of total FA in CX samples should not less than 1.25 mg·g-1 calculated on the dried basis. It was also found that the level of total FA was related to the quality, processing method and store duration of CX samples.


Li X.,Chengdu University of Traditional Chinese Medicine | Zhang L.-H.,Sichuan Provincial Institute for Food and Drug Control | Lv G.-H.,Chengdu University of Traditional Chinese Medicine | Wang X.-X.,Chengdu University of Traditional Chinese Medicine | And 3 more authors.
Zhongguo Zhongyao Zazhi | Year: 2013

Bioactivity of Danggui is linked to the content of ligustilide, but the relationship between ligustilide with herb shape, cultivating areas and plant species is still unknown. The relationship was investigated by quantifying on the amounts of Z-ligustilide and E-ligustilide by HPLC-DAD-MS method, and then comparing the content of ligustilides (the sum of Z-ligustilide and E-ligustilide) among forty-four various "Danggui" samples containing thirty Chinese Danggui (CDG), six Japanese Danggui (JDG), four Korea Danggui (KDG) and four European Danggui (EDG). Results showed that the content of ligustilides in CDG samples (Angelica sinensis) was in the range of 5.63-24.53 mg·g-1 with the mean of 11.02 mg·g-1(n=30). Ligustilides amounts were varied among samples cultivated in different areas in China, i.e. 13.90 mg·g-1 (n=6) in Yannan, 12.51 mg·g-1(n=6) in Sichuan and 10.04 mg·g-1(n=13) in Gansu. It was also found that ligustilides content was related to the shape, color and fragrance of herb, e.g. the relative larger amount of ligustilides was in the small main root, long rootlet and perfumed sample. Further, ligustilides contents were estimated to be 1.00 mg·g-1(n=6) in JDG samples (A. acutiloba and A. acutiloba var. sugiyamae) and 2.78 mg·g-1 (n=2) in EDG samples (lovage root, Levisticum officinale). However, ligustilides could not be detected in the four KDG samples (A. gigas) and two EDG samples (angelica root, A. archangelica). It has been concluded that ligustilide is significant variant among plant species, which may result in the variety of bioactivity and therapeutic effect.


Li X.-J.,University of Sichuan | Li X.-J.,Chengdu BaiKang Institute of Pharmacology and Toxicology | Yang K.,Chengdu BaiKang Institute of Pharmacology and Toxicology | du G.,Sichuan Provincial Institute for Food and Drug Control | And 3 more authors.
Analytical and Bioanalytical Chemistry | Year: 2015

A liquid chromatography–mass spectrometry (LC–MS) method coupled with specialized sample-preparation strategies was developed to investigate the hydrolysis of ginkgolide B (GB) in physiological environments in comparison with that of ginkgolide A (GA). The rapid hydrolysis processes were captured by the direct injection of samples prepared in the volatile buffers. The LC–MS behavior of the hydrolyzed products, including three monocarboxylates and three dicarboxylates, was acquired. The monocarboxylates were identified by fragmentation analysis, and the dicarboxylates were accordingly tentatively identified by reaction sequences. The base-catalyzed hydrolysis of GB and GA was characterized at 4 °C within pH 7.0–10.7. The regioselective reactions on the lactone-C and lactone-F were revealed by thermodynamic studies at pH 6.8 and 7.4. It was revealed that the 1-hydroxyl group on the skeleton of GB blocks the reactivity of the lactone-E. On the basis of these results, a distinctive hydrolysis phenomenon of GB was confirmed in plasma of humans, rats, and dogs as a rapid degradation of the trilactone along with the only production of the lactone-F-hydrolyzed product. This phenomenon is also closely associated with the 1-hydroxyl group, because it was not observed in GA. More interestingly, the underlying mechanism was revealed not to be associated with any typical enzyme-catalyzed process, but to be potentially involved with a selective reaction of the intact or broken lactone-C moiety with endogenous small-molecule reactants in plasma. This in-depth knowledge of the hydrolysis of GB versus GA not only facilitated understanding of their pharmacological mechanisms but also provided potential routes to study the structure–activity relationships of ginkgolides. [Figure not available: see fulltext.] © 2015 Springer-Verlag Berlin Heidelberg


Li X.-J.,University of Sichuan | Li X.-J.,Chengdu BaiKang Institute of Pharmacology and Toxicology | Yang K.,Chengdu BaiKang Institute of Pharmacology and Toxicology | Du G.,Sichuan Provincial Institute for Food and Drug Control | And 2 more authors.
Analytical and bioanalytical chemistry | Year: 2015

A liquid chromatography-mass spectrometry (LC-MS) method coupled with specialized sample-preparation strategies was developed to investigate the hydrolysis of ginkgolide B (GB) in physiological environments in comparison with that of ginkgolide A (GA). The rapid hydrolysis processes were captured by the direct injection of samples prepared in the volatile buffers. The LC-MS behavior of the hydrolyzed products, including three monocarboxylates and three dicarboxylates, was acquired. The monocarboxylates were identified by fragmentation analysis, and the dicarboxylates were accordingly tentatively identified by reaction sequences. The base-catalyzed hydrolysis of GB and GA was characterized at 4 °C within pH 7.0-10.7. The regioselective reactions on the lactone-C and lactone-F were revealed by thermodynamic studies at pH 6.8 and 7.4. It was revealed that the 1-hydroxyl group on the skeleton of GB blocks the reactivity of the lactone-E. On the basis of these results, a distinctive hydrolysis phenomenon of GB was confirmed in plasma of humans, rats, and dogs as a rapid degradation of the trilactone along with the only production of the lactone-F-hydrolyzed product. This phenomenon is also closely associated with the 1-hydroxyl group, because it was not observed in GA. More interestingly, the underlying mechanism was revealed not to be associated with any typical enzyme-catalyzed process, but to be potentially involved with a selective reaction of the intact or broken lactone-C moiety with endogenous small-molecule reactants in plasma. This in-depth knowledge of the hydrolysis of GB versus GA not only facilitated understanding of their pharmacological mechanisms but also provided potential routes to study the structure-activity relationships of ginkgolides. Graphical Abstract Regioselective hydrolysis of ginkgolide B in pH 7.4 buffers and plasma.


Wang A.-Q.,University of Sichuan | Wei B.-P.,Sichuan Provincial Institute for Food and Drug Control | Zhang Y.,University of Sichuan | Wang Y.-J.,University of Sichuan | And 2 more authors.
Journal of Chromatography B: Analytical Technologies in the Biomedical and Life Sciences | Year: 2011

For the endogenous substances with an ultra-low level in biological fluids, such as melatonin, the blank biological matrix is obviously not " blank" This problem leads to a serious issue of the bioanalytical methods development and validation by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS). This work developed and validated an ultra-high sensitive bioanalytical method for plasma melatonin by LC-MS/MS using water as calibration matrix. The lower limit of quantitation of the method was verified to be 1.0. pg/mL and the method exhibited a linear range of 1-5000. pg/mL. Potential matrix effects, accuracy and precision were fully monitored and validated by two complementary quality control approaches respectively using water and the pooled plasma as matrix. The intra-run and inter-run precisions were less than 11.5% and 12.2%, respectively, and the relative error was below ±13.8% for all of 5 quality control levels. The method was successfully applied to investigate the daytime (8:00. AM-8:00. PM) baseline level of endogenous plasma melatonin, as well as the pharmacokinetic profiles of exogenous melatonin after oral administration in beagle dogs. © 2011 Elsevier B.V.


Lan K.,University of Sichuan | Li X.-J.,University of Sichuan | Du G.,Sichuan Provincial Institute for Food and Drug Control | Xu L.,University of Sichuan
Journal of Pharmaceutical and Biomedical Analysis | Year: 2016

Ginkgolides are diterpenoid trilactones responsible for the neuromodulatory properties of Ginkgo biloba extracts. They are to be hydrolyzed in aqueous solutions as mixed carboxylate forms potentially including three monocarboxylates, three dicarboxylates and one tricarboxylate. Characterizations of the hydrolyzed products are challenging because there is no way to prepare them individually. In this work, the major hydrolyzed products of ginkgolide A (GA) and ginkgolide B (GB) including all three monocarboxyaltes have been produced in buffers and subjected to liquid chromatography coupled with triple quadrupole MS and LTQ Orbitrap MS analysis. With the comparative analysis of the trilactone of GA and GB, it was highlighted a unique charge-driven fragmentation pathway of twice neutral losses of CO on the lactone-C. The monocarboxylates were accordingly identified based on the construction of their fragmentation pathways cross-linked with those of the trilactone. In brief, the lactone-C hydrolyzed product is characteristic of the absence of product ions between [M-H]- and [M-H-C2H2O3]- (m/z 351 for GA and m/z 367 for GB). The featured fragmentation pathway of the lactone-F hydrolyzed product is the cleavage of ring-A, yielding a fragment (m/z 295 for GA and m/z 309 for GB) followed with twice (GA) or triple (GB) neutral losses of CO. The most characteristic fragment of the lactone-E hydrolyzed product is [M-H-H2O-CO2-2CO]- (m/z 307 for GA and m/z 323 for GB) in contrast to the other two monocarboxylates. The knowledge gained in this work was of special uses to investigate the biological fates and the corresponding pharmacological mechanisms of ginkgolides. © 2015 Elsevier B.V.


PubMed | Sichuan Provincial Institute for Food and Drug Control, University of Sichuan and Chengdu BaiKang Institute of Pharmacology and Toxicology
Type: Journal Article | Journal: Analytical and bioanalytical chemistry | Year: 2015

A liquid chromatography-mass spectrometry (LC-MS) method coupled with specialized sample-preparation strategies was developed to investigate the hydrolysis of ginkgolideB (GB) in physiological environments in comparison with that of ginkgolide A (GA). The rapid hydrolysis processeswere captured by thedirect injectionof samples prepared in the volatile buffers. The LC-MS behavior of the hydrolyzed products, including three monocarboxylates and three dicarboxylates, was acquired. The monocarboxylates were identified by fragmentation analysis, and the dicarboxylates were accordingly tentatively identified by reaction sequences. The base-catalyzed hydrolysis of GB and GA was characterized at 4C within pH7.0-10.7. The regioselective reactions on the lactone-C and lactone-F were revealed by thermodynamic studies at pH6.8 and 7.4. It was revealed that the 1-hydroxyl group on the skeleton of GB blocks the reactivity of the lactone-E. On the basis of these results, a distinctive hydrolysis phenomenon of GB was confirmed in plasma of humans, rats, and dogs as a rapid degradation of the trilactonealongwith the onlyproduction of the lactone-F-hydrolyzed product. This phenomenon is also closely associated with the 1-hydroxyl group, because it was not observed in GA. More interestingly, the underlying mechanism was revealed not to be associated with any typical enzyme-catalyzed process, but to be potentially involved with a selective reaction of the intact or broken lactone-C moiety with endogenous small-moleculereactants in plasma. This in-depth knowledge of the hydrolysis of GB versus GA not only facilitated understanding of their pharmacological mechanisms but also provided potential routes to study the structure-activity relationships of ginkgolides. Graphical Abstract Regioselective hydrolysis of ginkgolide B in pH 7.4 buffers and plasma.


PubMed | Sichuan Provincial Institute for Food and Drug Control and University of Sichuan
Type: | Journal: Journal of pharmaceutical and biomedical analysis | Year: 2015

Ginkgolides are diterpenoid trilactones responsible for the neuromodulatory properties of Ginkgo biloba extracts. They are to be hydrolyzed in aqueous solutions as mixed carboxylate forms potentially including three monocarboxylates, three dicarboxylates and one tricarboxylate. Characterizations of the hydrolyzed products are challenging because there is no way to prepare them individually. In this work, the major hydrolyzed products of ginkgolide A (GA) and ginkgolide B (GB) including all three monocarboxyaltes have been produced in buffers and subjected to liquid chromatography coupled with triple quadrupole MS and LTQ Orbitrap MS analysis. With the comparative analysis of the trilactone of GA and GB, it was highlighted a unique charge-driven fragmentation pathway of twice neutral losses of CO on the lactone-C. The monocarboxylates were accordingly identified based on the construction of their fragmentation pathways cross-linked with those of the trilactone. In brief, the lactone-C hydrolyzed product is characteristic of the absence of product ions between [M-H](-) and [M-H-C2H2O3](-) (m/z 351 for GA and m/z 367 for GB). The featured fragmentation pathway of the lactone-F hydrolyzed product is the cleavage of ring-A, yielding a fragment (m/z 295 for GA and m/z 309 for GB) followed with twice (GA) or triple (GB) neutral losses of CO. The most characteristic fragment of the lactone-E hydrolyzed product is [M-H-H2O-CO2-2CO](-) (m/z 307 for GA and m/z 323 for GB) in contrast to the other two monocarboxylates. The knowledge gained in this work was of special uses to investigate the biological fates and the corresponding pharmacological mechanisms of ginkgolides.


PubMed | Sichuan Provincial Institute for Food and Drug Control and Chengdu University of Traditional Chinese Medicine
Type: Comparative Study | Journal: Zhongguo Zhong yao za zhi = Zhongguo zhongyao zazhi = China journal of Chinese materia medica | Year: 2014

Bioactivity of Danggui is linked to the content of ligustilide, but the relationship between ligustilide with herb shape, cultivating areas and plant species is still unknown. The relationship was investigated by quantifying on the amounts of Z-ligustilide and E-ligustilide by HPLC-DAD-MS method, and then comparing the content of ligustilides (the sum of Z-ligustilide and E-ligustilide) among forty-four various Danggui samples containing thirty Chinese Danggui (CDG), six Japanese Danggui (JDG), four Korea Danggui (KDG) and four European Danggui (EDG). Results showed that the content of ligustilides in CDG samples (Angelica sinensis) was in the range of 5.63-24.53 mg x g(-1) with the mean of 11.02 mg x g(-1) (n = 30). Ligustilides amounts were varied among samples cultivated in different areas in China, i. e. 13.90 mg x g(-1) (n = 6) in Yannan, 12.51 mg x g(-1) (n = 6) in Sichuan and 10.04 mg x g(-1) (n = 13) in Gansu. It was also found that ligustilides content was related to the shape, color and fragrance of herb, e. g. the relative larger amount of ligustilides was in the small main root, long rootlet and perfumed sample. Further, ligustilides contents were estimated to be 1.00 mg x g(-1) (n = 6) in JDG samples (A. acutiloba and A. acutiloba var. sugiyamae) and 2.78 mg x g(-1) (n = 2) in EDG samples (lovage root, Levisticum officinale). However, ligustilides could not be detected in the four KDG samples (A. gigas) and two EDG samples (angelica root, A. archangelica). It has been concluded that ligustilide is significant variant among plant species, which may result in the variety of bioactivity and therapeutic effect.

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