1.Identification of chemical components of mahuang decoction by GC-MS and UPLC-Q-TOF-MS.
Rui LI ; Cen ZENG ; Ping WANG ; Xian-Li MENG ; Yong ZENG
China Journal of Chinese Materia Medica 2014;39(4):704-709
Since the polyjuice potion ingredient is complex, we need to develop an analysis method with well separation and high stability to perform qualitative analysis. After dividing chemical components of Mahuang Decoction into fat-soluble and water-soluble constituents by gradient extraction, GC-MS was used to analyze the chemical components of the ethyl acetate extraction. The results showed that forty compounds had been identified by NIST MS search 2.0 standard mass spectrometry Library and literatures. Next, UPLC-Q-TOF-MS was applied to idendify the chemical components of the water extraction. The results showed that thirty-nine compounds had been identified by MZmine-2.9.1, Isotope Pattern, fragmentation regularity of mass spectrometry and literatures. This experiment will provide evidences for elucidation of the effective substance in Mahuang decoction and can be used as a simple, shortcut method for analysis and identification for the polyjuice potion.
Chromatography, High Pressure Liquid
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methods
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Ephedra
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chemistry
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Ephedra sinica
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chemistry
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Gas Chromatography-Mass Spectrometry
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methods
2.Compatability chemistry of acid-alkaline pair medicine of Ephedra sinica and Glycyrrhiza uralencis in Maxing Shigan decoction.
Xiangping PEI ; Miaorong PEI ; Xiujun DUAN
China Journal of Chinese Materia Medica 2009;34(19):2466-2468
OBJECTIVETo investigate the change regularity of ephedrine and glyrihhzine acid in Ephedra sinila and Glycyrrhiza uralencis pair medicines and in Maxing Shigan decoction.
METHODThe contents of ephedrine and glycyrrhizic acid were determined by HPLC in samples of E. sinica extracts, G. uralencis extracts, pair medicines extracts of Maxing Shigao decoction sinica and G. uralencis, and extracts of E. sinica.
RESULTThere were no significant difference in ephedrine contents amoung different samples; the contents of glycyrrhizic acid were lower in decoctions of Maxing Shigan decoction than in G. uralencis decoction and pair medicines extracts.
CONCLUSIONMacromolecular complex was NOT formed by ephedrine and Glycyrrhizic acid in decoctions containing pair medicines of E. sinica and G. uralencis.
Chemistry, Pharmaceutical ; Drugs, Chinese Herbal ; chemistry ; Ephedra sinica ; chemistry ; Ephedrine ; chemistry ; Glycyrrhiza ; chemistry ; Glycyrrhizic Acid ; chemistry
3.Study on multi-target optimization of prescription dose of Mahuang decoction.
Yu HE ; Yu-Quan GAI ; Hui-Fen ZHOU ; Yan-Wen SUN ; Wei-Feng JIN ; Hai-Tong WAN
China Journal of Chinese Materia Medica 2014;39(7):1270-1275
OBJECTIVETo optimize the prescription dose of Mahuang decoction in a multi-target manner, in order to provide reference for the quantitative optimization of the prescription dose of the traditional Chinese medicine compound.
METHODThe number of diaphoretic spots in rats, the tracheal antispasmodic rate in guinea pigs and the writhing times by acetic acid in mice were taken as the indexes for evaluating the diaphoretic, antispasmodic and analgesic effects. According to the experimental results of the 16 orthogonal combination prescriptions, a mathematical dose-effect model was built by support vector regression (SVR) and quadratic response surface regression (RSR) respectively. The multi-target optimization was achieved by elitist non-dominated sorting genetic algorithm (NSGA-II) and entropy weight TOPSIS method.
RESULTThe optimal dose of Mahuang decoction after being optimized by SVR modeling contained 17.71 g of Ephedrae Herba, 9.57 g of Cinnamomi Ramulus, 11.75 g of Armeniacae Semen Amarum and 4.39 g of Glycyrrhizae Radix et Rhizoma Praeparata Cum Melle. The optimized result by RSR modeling contained 13.37 g of Ephedrae Herba, 11.61 g of Cinnamomi Ramulus, 11.98 g of Armeniacae Semen Amarum and 5.67 g of Glycyrrhizae Radix et Rhizoma Praeparate Cum Melle. SVR was superior to RSR in both of the forecast capacity and optimization results.
CONCLUSIONSVR-NSGA-II-TOPSIS method could be adopted for the multi-target optimization for the dose of Mahuang decoction and other traditional Chinese medicine compounds. It is proved to be the optimal prescription with the best efficacy, and could provide scientific quantitative basis for determining the dose of traditional Chinese medicine compound prescriptions and developing new traditional Chinese medicines.
Animals ; Cinnamomum ; chemistry ; Drug Compounding ; methods ; Drug Dosage Calculations ; Drug Prescriptions ; Ephedra ; chemistry ; Ephedra sinica ; chemistry ; Glycyrrhiza ; chemistry ; Guinea Pigs ; Mice ; Rats
4.In vitro microdialysis recoveries of nine active ingredients in Mahuang decoction.
Ying-hong TANG ; Hai-tong WAN ; Jian-zhen CHEN ; Hui-fen ZHOU ; Yan-fang TIAN ; Yu HE
China Journal of Chinese Materia Medica 2015;40(18):3667-3673
To detect the in vitro probe microdialysis recoveries based on an HPLC-DAD method for simultaneous quantification of nine active ingredients (ephedrine, pseudoephedrine, methylephedrine, amygdalin, liquiritin, cinnamyl alcohol, cinnamic acid, cinnamaldehyde and glycyrrhizic acid) in Mahuang decoction, which provides reference for in vivo pharmacokinetic study. The concentrations of nine active ingredients in dialysate were detected by HPLC-DAD, to investigate the effect of flow rates (incremental method and subtraction method) and intraday stability of the probe recoveries and medium concentrations on the recoveries. Nine active ingredients could be well separated in 52 min. At the perfusion rate of 1.0 μL x min(-1), the relative recoveries of ephedrine, pseudoephedrine, methylephedrine, amygdalin, liquiritin, cinnamyl alcohol, cinnamic acid, cinnamaldehyde and glycyrrhizic acid were (50.95 ± 0.82)%, (52.74 ± 1.13)%, (51.29 ± 0.51)%, (32.56 ± 0.84)%, (45.36 ± 0.83)%, (70.94 ± 0.99)%, (69.98 ± 2.30)%, (71.68 ± 0.63)%, and (22.14 ± 0.48)%, respectively. And the probe kept steady in 7 hours. At the same medium concentration, the probe recoveries decreased exponentially with the increase in flow rates. The recoveries of seven ingredients detected by these two methods were similar at certain flow rates, except for amygdalin and cinnamaldehyde. At the same flow rate, the relative recoveries of cinnamyl alcohol, cinnamic acid and cinnamaldehyde changed greatly (9.55%-16.2%) and the others six ingredients had less change (3.27%-5.71%) with the changes in medium concentrations. Microdialysis method could be used to detect the in vitro recoveries of nine ingredients in Mahuang decoction. Reverse dialysis method could be used for the in vivo probe recovery calibration of ephedrine, pseudoephedrine, methylephedrine, liquiritin, cinnamyl alcohol and cinnamic acid at the flow rate of 2.0 μL x min(-1).
Chromatography, High Pressure Liquid
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Drugs, Chinese Herbal
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chemistry
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isolation & purification
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Ephedra sinica
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chemistry
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Microdialysis
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methods
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Molecular Structure
5.Determination of ephedrine and pseudoephedrine in Herba Ephedrae and Maxing Shigan Tang by capillary zone electrophoresis.
Haoran JING ; Huaizhong GUO ; Zijun WANG ; Min WANG ; Bin ZHANG
China Journal of Chinese Materia Medica 2009;34(8):980-983
OBJECTIVETo establish a method for the determination of ephedrine and pseudoephedrine in Herba Ephedrae and Maxing Shigan Tang by capillary zone electrophoresis.
METHODThe conditions of the experiment were optimized with a fused-silica capillary of 60 cm x 50 microm (50 cm effective length) in a running buffer of 50 mmol x L(-1) borax-20 mmol x L(-1) threonine (pH 9.27) and an applied voltage of 15 kV (room temperature). Samples were introduced by hydrodynamic injections (10 cm x 20 s)and determined with on-column UV monitoring at 210 nm. Phenobarbital was chosen as the internal standard.
RESULTEphedrine and pseudoephedrine are separated successfully within 8 min. The linear responses covered the ranges from 21.3 to 213 mg x L(-1) (r = 0.9996) for ephedrine and from 8.4 to 84 mg x L(-1) (r = 0.9995) for pseudoephedrine. The detection limits (S/N = 3) of ephedrine and pseudoephedrine were shown to be 1.45 and 1.48 microg x mL(-1), respectively, The quantitation limits (S/N = 10) of ephedrine and pseudoephedrine were shown to be 4.81 and 4.93 mg x L(-1), respectively. The average recoveries for ephedrine and pseudoephedrine were 97.5% and 98.6% with RSD less than 5.0%.
CONCLUSIONThe method is simple, rapid, cost-effective and precise with satisfactory results.
Drugs, Chinese Herbal ; Electrophoresis, Capillary ; methods ; Ephedra sinica ; chemistry ; Ephedrine ; analysis ; Plants, Medicinal ; chemistry ; Pseudoephedrine ; analysis ; Reproducibility of Results
6.Pharmacokinetics of compatible effective components of Mahuang Decoction in febrile rats.
Jia-Yang WAN ; Yan-Fang TIAN ; Hai-Tong WAN ; Li YU ; Hui-Fen ZHOU ; Chang LI ; Yu HE
China Journal of Chinese Materia Medica 2019;44(10):2149-2155
In the present paper,after the febrile rat model was prepared by injecting yeast,orthogonally compatible effective components from prescription drugs of Mahuang Decoction( Ephedra sinica total alkaloids,Cinnamomum cassia essential oil,amygdalin,Glycyrrhiza uralensis total flavonoids+G. uralensis total saponins) with nine different dosage ratios were given by gavage administration.The plasma concentrations of main active ingredients including ephedrine hydrochloride,pseudoephedrine hydrochloride,methylephedrine hydrochloride,cinnamic acid,amygdalin,liquritin and glycyrrhizin at different time points were analyzed by liquid chromatograph mass spectrometer( LC-MS). Based on the pharmacokinetic parameters of non-compartmental model,the area under curve of total quantum( AUCt) and the mean chromatographic retention time of total quantum( MRTt) were further calculated,in order to evaluate the effect of compatibility on the total statistical moment parameters. The results showed that the pharmacokinetic characteristics of main active components in febrile rats were significantly different after treatment with orthogonally compatibility of E. sinica total alkaloids,C.cassia essential oil,amygdalin,G. uralensis total flavonoids and G. uralensis total saponins. Orthogonal analysis confirmed that different compatibility components had different effects on the total statistical moment parameters. The contribution of effective components of Mahuang Decoction to AUCtwas as follows in a descending order: E. sinica total alkaloids>C. cassia essential oil>amygdalin>G. uralensis total flavonoids+G. uralensis total saponin,while the contribution to MRTtwas: E. sinica total alkaloids >G. uralensis total flavonoids+G. uralensis total saponin>amygdalin>C. cassia essential oil. The E. sinica total alkaloid had the greatest effects on both of the above parameters,and the optimal combination was A_3B_3C_2D_1 for AUCt,and A_1B_1C_1D_1 for MRTt.
Animals
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Drugs, Chinese Herbal
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pharmacokinetics
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Ephedra sinica
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chemistry
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Glycyrrhiza uralensis
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chemistry
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Oils, Volatile
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pharmacokinetics
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Phytochemicals
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pharmacokinetics
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Rats
7.Analysis of essential oil in herba ephedrae-ramulus cinnamomi by GC-MS and chemometric resolution method.
Xiao-ru LI ; Yi-zeng LIANG ; Xiao-ning LI
Acta Pharmaceutica Sinica 2007;42(2):187-191
Gas chromatography/mass spectrometry, chemometric resolution method ( CRM) and overall volume integration method were used to analyze the essential components of herbal pair Herba Ephedrae-Ramulus Cinnamomi (HP HE-RC) and compare it with that of single herbs HE and RC. 72, 68, and 97 essential components in essential oil of HE, RC, and HP HE-RC were determined, accounting for 90. 08% , 91. 62% , and 89. 76% of total contents of essential oil of HE, RC, and HP HE-RC, respectively. The numbers of essential components of HP HE-RC are almost the summation of that of two single herbs, but some relative contents of them are changed. Some new components, such as 1, 6-dimethylhepta-1,3,5-triene, tetracyclo[4. 2. 1.1 (2,5 ). 0 (9,10) ] deca-3,7-diene, globulol, ( E, E) -6, 10,14-trimethyl-5,9,13-pentadecatrien-2 -one, etc. have been found in HP HE-RC because of chemical reactions and physical changes during the course of decocation.
Chemistry Techniques, Analytical
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methods
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Cinnamomum
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chemistry
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Drug Combinations
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Ephedra sinica
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chemistry
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Gas Chromatography-Mass Spectrometry
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methods
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Oils, Volatile
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analysis
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chemistry
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Plant Oils
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analysis
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chemistry
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Reproducibility of Results
8.Comparative analysis of volatile oils in the stems and roots of Ephedra sinica via GC-MS-based plant metabolomics.
Meng-Ying LV ; Jian-Bo SUN ; Min WANG ; Hong-Yan FAN ; Zun-Jian ZHANG ; Feng-Guo XU
Chinese Journal of Natural Medicines (English Ed.) 2016;14(2):133-140
With a great difference in therapeutic effects of Mahuang (MH, the stems of Ephedra sinica) and Mahuanggen (MHG, the roots of Ephedra sinica), chemical differences between MH and MHG should be investigated. In the present study, gas chromatography-mass spectrometry (GC-MS)-based plant metabolomics was employed to compare volatile oil profiles of MH and MHG. The antioxidant activities of volatile oils from MH and MHG were also compared. 32 differential chemical markers were identified according to the variable importance in the projection (VIP) value of orthogonal partial least squares discriminant analysis (OPLS-DA) and P value of Mann-Whitney test. Among them, chemical markers of tetramethylpyrazine (TMP) and α-terpineol were quantified. Their contents were much higher in most MH samples compared with MHG. The antioxidant assay demonstrated that MH had significantly higher free radical-scavenging activity than MHG. Although MH and MHG derived from the same medicinal plant, there was much difference in their volatile oil profiles. MH samples had significantly higher content of two reported pharmacologically important chemical markers of TMP and α-terpineol, which may account for their different antioxidant activities.
Drugs, Chinese Herbal
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chemistry
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Ephedra sinica
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chemistry
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Gas Chromatography-Mass Spectrometry
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Metabolomics
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Oils, Volatile
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chemistry
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Plant Roots
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chemistry
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Plant Stems
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chemistry
9.Study on residue analysis method of imidacloprid in Ephedrae sinica.
Mei-yan CHEN ; Jun CHEN ; Jian XUE ; Jing YU ; Hui-zhen CHENG
China Journal of Chinese Materia Medica 2007;32(8):675-677
OBJECTIVETo establish residue analysis method of imidacloprid in Ephedra sinica by HPLC.
METHODImidacloprid was extracted with dichloromethane, cleaned up with chromatography column, then separated on Spherisorb C18 column by using Methanol-water (20:80), detected at 270 nm.
RESULT AND CONCLUSIONThe limit of detection (LOD) and limit quantification (LOQ) were 0.4 x 10(-9) g and 0.02 mg x kg(-1), mean recovery and related standard deviation (RSD) were 85.37%-90.65% and 2.23%-3.45%. It is concluded that the method could satisfy the pesticide residue analysis demands in sensitivity, accuracy and precision.
Chromatography, High Pressure Liquid ; methods ; Ephedra sinica ; chemistry ; Imidazoles ; analysis ; Insecticides ; analysis ; Neonicotinoids ; Nitro Compounds ; analysis ; Pesticide Residues ; analysis ; Plants, Medicinal ; chemistry ; Reproducibility of Results
10.A Case of Ischemic Colitis Associated with the Herbal Food Supplement Ma Huang.
Hyun Joo SONG ; Ki Nam SHIM ; Kum Hei RYU ; Tae Hun KIM ; Sung Ae JUNG ; Kwon YOO
Yonsei Medical Journal 2008;49(3):496-499
Ischemic colitis is a condition that usually occurs in the elderly, as a form of vascular disease. However, ischemic colitis also occurs, though rarely, in healthy young adults. Moreover, food supplements containing Ephedra sinica or ma huang have been linked to adverse central nervous and cardiovascular events. A 40-year-old man was admitted to our emergency department after 2 episodes of abdominal pain and bloody diarrhea that lasted 24 hours. His medical history was unremarkable for risk factors of bowel ischemia, except for well-controlled hypertension. However, a weight-loss supplement, Ephedra sinica, had been prescribed for daily use during the previous month. Both abdominal/pelvic computed tomography and colonoscopy revealed findings compatible with ischemic colitis. His conditions spontaneously improved without any serious complications, and he was advised to discontinue the use of herbal medications containing ephedrine. In this paper, we describe a case of ischemic colitis that was potentially linked to the use of ma huang with a review of the relevant literature.
Abdominal Pain/etiology
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Adult
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Colitis, Ischemic/*diagnosis/etiology
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Diarrhea/etiology
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*Dietary Supplements
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Drugs, Chinese Herbal/administration & dosage/adverse effects
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Ephedra sinica/*chemistry
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Humans
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Male