CN103698416B - Determination method of contents of saccharate and saccharic acid 1,4-lactone in Liuwei Dihuang preparations - Google Patents
Determination method of contents of saccharate and saccharic acid 1,4-lactone in Liuwei Dihuang preparations Download PDFInfo
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Abstract
The invention belongs to the field of pharmaceutical analysis, and relates to a determination method of contents of saccharate and saccharic acid 1,4-lactone, two newly-discovered pharmacologically-active components, in Chinese patent medicine Liuwei Dihuang series preparations. According to the invention, saccharic acid (saccharate) and (or) saccharic acid 1,4-lactone in Liuwei Dihuang preparations are extracted by a Na2CO3 solution or a 60% methanol solution. The two compounds are analyzed quantitatively by separating detection technologies such as hydrophilic chromatography HPLC-HILIC-UV/ELSD/MS, and the like. The invention establishes the determination method of contents of saccharate and its lactone in Liuwei Dihuang preparations for the first time, and provides a new thinking and method for quality control of Liuwei Dihuang preparations.
Description
Technical field
The present invention relates to Pharmaceutical Analysis field, particularly the content assaying method of glucarate and glucaric acid Isosorbide-5-Nitrae lactone in six drugs containing rehmanniae preparation series.
Background technology
Liuwei Dihuang Wan by the 6 taste Chinese medicines such as prepared rhizome of rehmannia, the fruit of medicinal cornel, Chinese yam, rhizoma alismatis, moutan bark, Poria cocos according to a certain percentage compatibility form, the clinical practice history of existing centuries is the classics recipe of traditional Chinese medicine.Along with deepening continuously of clinical research, it cures mainly and is also extended to inside and outside, woman, youngster, face Deng Ge section by original pediatric drugs, relates to illness and has reached more than 40 and plant, have good curative effect especially to complicated chronic disease etc.Due to this patent medicine determined curative effect, almost there is no Reporting of harms, and the factor such as cheap, dark in popular favor.At present, about there are upper hundred manufacturer production six drugs containing rehmanniae products at home, mainly contain decoction, pill, oral liquid and capsule etc.; Have tens six drugs containing rehmanniae brands, annual sales amount, more than 1,000,000,000 yuan, has good Social benefit and economic benefit.
The methods such as applied chemistry and pharmacology combine, serum drug chemistry are to the pharmacological component of Liuwei Dihuang Wan, enter blood and internal metabolism composition etc. and carry out comparatively deep research, separation has obtained some bioactive polysaccharide or small molecule metabolite, achieves gratifying achievement.Metabolism group (metabonomics) is new ' group is learned ' technology occurred after genomics, transcriptomics and proteomics, under the condition mainly biosome stimulated at pathologic, physiologic, in the change of different time, multi-faceted quantitative its metabolite content of detection, inquire into and intervene thing to the subject of the regulatory mechanism of body.In recent years, metabolism group in discovery to medical diagnosis on disease, treat that relevant metabolic marker thing is studied, all have a wide range of applications in medicine effect and toxicity assessment, mechanism of action etc., demonstrate huge potentiality.We are on the basis of identifying based on HPLC-UV metabolism group Characteristic chromatographic peak, by the relative variation relation to 4 Characteristic chromatographic peaks, infer that Liuwei Dihuang Wan may affect the activity of beta-glucuronidase enzyme in rat body.Confirm that Liuwei Dihuang Wan has obvious beta-glucuronidase enzyme inhibition through experiment in vivo and vitro, thus found an action target spot---the beta-glucuronidase enzyme of Liuwei Dihuang Wan.On this basis, by being progressively separated the method that Liuwei Dihuang Wan chemical composition and vitro enzyme determination of activity combine, find and identify a kind of new pharmacological component-glucaric acid Isosorbide-5-Nitrae lactone in Liuwei Dihuang Wan.Literature research (Charles B.S., Journal of Orthomolecular Medicine Vol. 16, No. 2,2001) show that this material (comprising its precursor glucarate) has and comprise anticancer and that estrogen is relevant pharmacological action widely, before, this compound does not have the report be found in Chinese herbal medicine, therefore, does not have glucarate and lactone thereof at the report of Chinese herbal medicine content assaying method.
Although glucarate is found to be present in fruit as in apple and grape and a small amount of vegetables, up to now, has no and utilize HPLC-HILIC-UV/ELSD and HPLC-MS/MS technology to carry out the report of quantitative measurement to them.
Summary of the invention
Fundamental purpose of the present invention applies multiple separation detection technique such as HPLC-HILIC-UV/ELSD/MS to the new discovery component sugar glucose diacid salt in six drugs containing rehmanniae preparation series and glucaric acid Isosorbide-5-Nitrae lactone to carry out quantitative test.
Glucarate and glucaric acid Isosorbide-5-Nitrae lactone structure formula as follows:
Concrete scheme of the present invention is as follows:
Take a certain amount of Liuwei Dihuang preparation, add 60% methanol solution of certain volume, ultrasonic 20min, centrifugal, precipitation is extracted once with the above-mentioned solution of equal-volume again, centrifugal, merges supernatant; Gained supernatant is directly analyzed by MS or HPLC-MS technology; Glucarate characteristic molecular negative ion quasi-molecular ions is 209,191,85; Glucaric acid Isosorbide-5-Nitrae lactone characteristic molecular negative ion quasi-molecular ions is 191,85; Chromatographic retention, mass spectrogram are consistent with standard items.
Glucarate and glucaric acid Isosorbide-5-Nitrae lactone content assay method in Liuwei Dihuang preparation, comprising:
1) glucarate and glucaric acid 1, the preparation of 4 lactone standard solution: precision takes glucarate and glucaric acid 1 respectively, 4 lactone two kinds reference substance 40.0mg, quantitatively be transferred in 10.0mL volumetric flask, thin up is to scale, and precision pipettes in 5.0mL to 10.0mL volumetric flask, adds 80% dilution in acetonitrile to scale, be mixed with 200.0ug/mL solution, in contrast product mother solution;
2) HPLC-HILIC-UV/ELSD method measures the content of total glucarate in Liuwei Dihuang Wan:
Get Liuwei Dihuang Wan, pulverize, precision takes 500mg, adds 4Ml 2-5%Na
2cO
3the ultrasonic 20min of solution, centrifugal, precipitation is extracted once with the above-mentioned solution of equal-volume again, centrifugal, merges supernatant; Adopt the little column extracting of C18 SPE, collect 5% methanol-eluted fractions, with the 55 DEG C of dryings of high-speed vacuum centrifugal drier, dry thing accurately adds 1.0mL 80% acetonitrile, 10,000 leaves heart 10min gets supernatant and carries out HPLC-HILIC-UV/ELSD analysis, carries out quantitatively with calibration curve method to glucarate; HPLC-HILIC-UV method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC, internal diameter 4.6mm, granularity 5um; With acetonitrile-5mM ammonium dihydrogen phosphate (ADP) for mobile phase, both volume ratios are 78:22 perseverance degree wash-out; Flow velocity 0.8mL/min; Determined wavelength 205nm; Sample introduction 10ul, column temperature 30 DEG C; HPLC-HILIC-ELSD method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC ZIC-HILIC, internal diameter 4.6mm, granularity 5um; Be eluent gradient wash-out with acetonitrile A phase-0.02% Ammoniom-Acetate B phase: 0-5min A phase 80%, 5-25min A phase 80%-75%, 25-30min A phase is 75%-50%, 30-35min A phase is 50%-80%; Flow velocity 0.8mL/min; Sample introduction 10ul, drift tube temperature 60 DEG C of air-flow 1.2L/min;
3) in Liuwei Dihuang Wan, glucaric acid Isosorbide-5-Nitrae lactone content measures:
Get Liuwei Dihuang Wan, pulverize, precision takes 500mg, add 4.0 mL 60% methanol solutions, ultrasonic 20min, 5,000 leaves heart 10min gets supernatant, and residue continues to add 4.0mL 60% methanol solution, ultrasonic 20min, 5,, 000 leaves heart 10min gets supernatant, merges supernatant, 14,000 to leave after the heart suitably dilution sample introduction UPLC-MS/MS analyzes; Chromatographic condition: Waters BEH C18 chromatographic column, long 50mm, internal diameter 1.0 mm, particle diameter 1.7um, column temperature: 40 DEG C; Mobile phase: A phase is 10mM formic acid, B phase is acetonitrile; Flow velocity 0.4mL/min; Mass Spectrometry Conditions: Negative electrospray ionization source ESI-, voltage 2000V, source temp 100 DEG C, taper hole voltage 15V, desolventizing temperature degree 300 DEG C, taper hole gas and desolventizing airshed are respectively 50 and 600L/min; Full scan pattern 50 ~ 1200amu; Secondary collision energy 15V; The intensity of the fragment peak 85 of molecular ion peak 191 is used for the quantitative of glucose 1.4-lactone; Carry out quantitatively with calibration curve method to glucaric acid Isosorbide-5-Nitrae lactone;
4) in Liuwei Dihuang Wan, glucarate and glucaric acid Isosorbide-5-Nitrae lactone detect simultaneously:
Get Liuwei Dihuang Wan, pulverize, precision takes 500mg, add 4.0 mL 60% methanol solutions, ultrasonic 20min, 5,000 leaves heart 10min gets supernatant, and residue continues to add 4.0mL 60% methanol solution, ultrasonic 20min, 5,, 000 leaves heart 10min gets supernatant, merges supernatant, 14,000 to leave after the heart suitably dilution sample introduction HPLC-LILIC-UV analyzes; HPLC-HILIC-UV method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC, internal diameter 4.6mm, granularity 5um; With acetonitrile A phase-5mM ammonium dihydrogen phosphate (ADP)+1.0% phosphoric acid B phase for mobile phase, eluent gradient elution program: 0-3min A phase 83%, 3-15min A phase 83-65%, 15-18min A phase 65%, 18-20min A phase 65-83%, 20-30min A phase 83%; Determined wavelength 205nm; Sample introduction 10ul, column temperature 30 DEG C; With calibration curve method, simultaneous quantitative is carried out to glucarate and glucaric acid Isosorbide-5-Nitrae lactone.
Described Na
2cO
3solution concentration is preferably 2.0%.
The invention has the beneficial effects as follows: in view of the new discovery component sugar glucose diacid salt in six drugs containing rehmanniae preparation series and glucaric acid 1,4 lactones have clear and definite action target spot and pharmacological action widely, and the present invention applies the quality control, effective substance research etc. that the quantitative analysis method of multiple separation detection technique as HPLC-HILIC-UV/ELSD/MS contributes to six drugs containing rehmanniae preparation series.
Accompanying drawing explanation
Fig. 1 HPLC-HILIC-UV method measures total glucarate chromatogram in Liuwei Dihuang Wan
A: glucaric acid potassium standard items chromatogram.B: Liuwei Dihuang Wan 2.0%Na2CO3 extract chromatogram.
Fig. 2 HPLC-HILIC-ELSD method measures total glucarate chromatogram in Liuwei Dihuang Wan
A: Liuwei Dihuang Wan 2.0%Na2CO3 extract chromatogram.B: glucaric acid potassium standard items chromatogram.
Fig. 3 UPLC-MS/MS method measures glucaric acid Isosorbide-5-Nitrae lactone chromatogram in Liuwei Dihuang Wan
A: glucaric acid Isosorbide-5-Nitrae lactone standard items chromatogram.B: Liuwei Dihuang Wan 60% methanol extract liquid chromatogram.
Glucarate and glucaric acid Isosorbide-5-Nitrae lactone chromatogram in Fig. 4 HPLC-HILIC-UV method Simultaneously test Liuwei Dihuang Wan
A: Liuwei Dihuang Wan 60% methanol extract liquid adds glucaric acid potassium and glucaric acid Isosorbide-5-Nitrae lactone standard items chromatogram.B: Liuwei Dihuang Wan 60% methanol extract liquid chromatogram.C: glucaric acid potassium and glucaric acid Isosorbide-5-Nitrae lactone standard items chromatogram.
Embodiment
embodiment 1
HPLC-HILIC-UV/ELSD method measures the content of total glucarate in Liuwei Dihuang Wan
1) glucaric acid Isosorbide-5-Nitrae lactone changes into glucarate
Respectively with the Na of variable concentrations
2cO
3solubilize preparation glucaric acid Isosorbide-5-Nitrae lactone standard items, HPLC-HILIC-UV analyzes, and determines that glucaric acid Isosorbide-5-Nitrae lactone is converted into the condition of glucarate completely.The Na of result display 2.0%
2cO
3solution can make glucaric acid Isosorbide-5-Nitrae lactone be converted into glucarate completely completely.
2) assay
Get Liuwei Dihuang Wan (Beijing Tongrentang, condensed pill), pulverize, precision takes 500mg, adds 4.0Ml 2% Na
2cO
3the ultrasonic 20min of solution, centrifugal, precipitation is extracted once with the above-mentioned solution of equal-volume again, centrifugal, merges supernatant; Adopt C18 SPE little column extracting, collect 5% methanol-eluted fractions, with the 55 DEG C of dryings of high-speed vacuum centrifugal drier, dry thing accurately adds 1.0mL 80% acetonitrile, and 10,000 leaves heart 10min gets supernatant and carry out HPLC-HILIC-UV/ELSD analysis.
HPLC-HILIC-UV method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC, internal diameter 4.6mm, granularity 5um.With acetonitrile-5mM ammonium dihydrogen phosphate (ADP) for mobile phase, both volume ratios are 78:22 perseverance degree wash-out.Flow velocity 0.8mL/min; Determined wavelength 205nm; Sample introduction 10ul, column temperature 30 DEG C.Typical color spectrogram is as Fig. 1
.record in three batches of Liuwei Dihuang Wans (condensed pill, Beijing Tongrentang) containing total glucarate be 8.0-10.0mg/g.
HPLC-HILIC-ELSD method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC ZIC-HILIC, internal diameter 4.6mm, granularity 5um.With acetonitrile (A)-0.02% Ammoniom-Acetate (B) for eluent gradient wash-out: 0-5min A phase 80%, 5-25min A phase 80%-75%, 25-30min A phase is 75%-50%, 30-35min A phase is 50%-80%.Flow velocity 0.8mL/min; Sample introduction 10ul, drift tube temperature 60 DEG C of air-flow 1.2L/min.
typical color spectrogram is as Fig. 2.record in three batches of Liuwei Dihuang Wans (condensed pill, Beijing Tongrentang) containing total glucarate be 8.6-11.2mg/g.
embodiment 2
UPLC-MS/MS method measures the content of glucose 1.4-lactone in Liuwei Dihuang Wan
Get Liuwei Dihuang Wan (Beijing Tongrentang, condensed pill), pulverize, precision takes 500mg, adds 4.0 mL 60% methanol solutions, ultrasonic 20min, 5,000 leaves heart 10min gets supernatant, and residue continues to add 4.0mL 60% methanol solution, ultrasonic 20min, 5,000 leaves heart 10min gets supernatant, merge supernatant, 14,000 to leave after the heart suitably dilution sample introduction UPLC-MS/MS analyzes.
Chromatographic condition: Waters BEH C18 chromatographic column, long 50mm, internal diameter 1.0 mm, particle diameter 1.7um, column temperature: 40 DEG C.Mobile phase: A phase is 10mM formic acid, B phase is acetonitrile; Flow velocity 0.4mL/min.Mass Spectrometry Conditions: Negative electrospray ionization source (ESI-), voltage 2000V, source temp 100 DEG C, taper hole voltage 15V, desolventizing temperature degree 300 DEG C, taper hole gas and desolventizing airshed are respectively 50 and 600L/min.Full scan pattern (50 ~ 1200amu).Secondary collision energy 15V.The intensity of the fragment peak 85 of molecular ion peak 191 is used for the quantitative of glucose 1.4-lactone.With calibration curve method, glucaric acid Isosorbide-5-Nitrae lactone is carried out quantitatively.Typical color spectrogram is as Fig. 3. this method record in 3 batches of Liuwei Dihuang Wans (condensed pill, Beijing Tongrentang) containing glucaric acid Isosorbide-5-Nitrae lactone be 3.5-5.0mg/g.
embodiment 3
The content of glucarate and glucose 1.4-lactone in HPLC-LILIC-UV method Simultaneously test Liuwei Dihuang Wan
Get Liuwei Dihuang Wan (Beijing Tongrentang, condensed pill), pulverize, precision takes 500mg, adds 4.0 mL 60% methanol solutions, ultrasonic 20min, 5,000 leaves heart 10min gets supernatant, and residue continues to add 4.0mL 60% methanol solution, ultrasonic 20min, 5,000 leaves heart 10min gets supernatant, merge supernatant, 14,000 to leave after the heart suitably dilution sample introduction HPLC-LILIC-UV analyzes.
HPLC-HILIC-UV method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC, internal diameter 4.6mm, granularity 5um.With acetonitrile (A)-5mM ammonium dihydrogen phosphate (ADP)+1.0% phosphoric acid (B) for mobile phase, eluent gradient elution program: 0-3min A phase 83%, 3-15min A phase 83-65%, 15-18min A phase 65%, 18-20min A phase 65-83%, 20-30min A phase 83%.Determined wavelength 205nm; Sample introduction 10ul, column temperature 30 DEG C.Typical color spectrogram is as Fig. 4.With calibration curve method, glucarate and glucaric acid Isosorbide-5-Nitrae lactone are carried out quantitatively.Record in 3 batches of Liuwei Dihuang Wans (condensed pill, Beijing Tongrentang) and contain total glucarate at 2.0-4.8mg/g, containing glucaric acid Isosorbide-5-Nitrae lactone at 4.0-6.5mg/g.
The glucarate that the present invention sets up and (or) glucaric acid Isosorbide-5-Nitrae lactone quantitative detecting method meets the requirement of Chinese Pharmacopoeia (2010 editions) to chromatographic fractionation system adaptability, accuracy, linear relationship and precision.
The above is only the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, without departing from the inventive concept of the premise; can also make some improvements and modifications, these improvements and modifications also should be considered within the scope of protection of the present invention.
Claims (2)
1. glucarate and glucaric acid 1 in Liuwei Dihuang preparation, 4 lactone content assay methods, it is characterized in that comprising: 1) glucarate and glucaric acid 1, the preparation of 4 lactone standard solution: precision takes glucarate and glucaric acid 1 respectively, 4 lactone two kinds reference substance 40.0mg, quantitatively be transferred in 10.0mL volumetric flask, thin up is to scale, precision pipettes in 5.0mL to 10.0mL volumetric flask, add 80% dilution in acetonitrile to scale, be mixed with 200.0 μ g/mL solution, in contrast product mother solutions;
2) HPLC-HILIC-UV/ELSD method measures the content of total glucarate in Liuwei Dihuang Wan:
Get Liuwei Dihuang Wan, pulverize, precision takes 500mg, adds 4.0mL 2-5%Na
2cO
3the ultrasonic 20min of solution, centrifugal, precipitation is extracted once with the above-mentioned solution of equal-volume again, centrifugal, merges supernatant; Adopt the little column extracting of C18 SPE, collect 5% methanol-eluted fractions, centrifugal with high-speed vacuum, dryer 55 DEG C of dryings, dry thing accurately adds 1.0mL 80% acetonitrile, 10,000 leaves heart 10min gets supernatant and carries out HPLC-HILIC-UV/ELSD analysis, carries out quantitatively with calibration curve method to glucarate; HPLC-HILIC-UV method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC, internal diameter 4.6mm, granularity 5 μm; With acetonitrile-5mM ammonium dihydrogen phosphate (ADP) for mobile phase, both volume ratios are 78:22 perseverance degree wash-out; Flow velocity 0.8mL/min; Determined wavelength 205nm; Sample introduction 10 μ l, column temperature 30 DEG C; HPLC-HILIC-ELSD method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC ZIC-HILIC, internal diameter 4.6mm, granularity 5 μm; Be eluent gradient wash-out with acetonitrile A phase-0.02% Ammoniom-Acetate B phase: 0-5min A phase 80%, 5-25min A phase 80%-75%, 25-30min A phase is 75%-50%, 30-35min A phase is 50%-80%; Flow velocity 0.8mL/min; Sample introduction 10 μ l, drift tube temperature 60 DEG C, air-flow 1.2L/min;
3) in Liuwei Dihuang Wan, glucaric acid Isosorbide-5-Nitrae lactone content measures:
Get Liuwei Dihuang Wan, pulverize, precision takes 500mg, add 4.0 mL 60% methanol solutions, ultrasonic 20min, 5,000 leaves heart 10min gets supernatant, residue continues to add 4.0mL 60% methanol solution, ultrasonic 20min, 5000 leave heart 10min gets supernatant, merges supernatant, 14,000 to leave after the heart suitably dilution sample introduction UPLC-MS/MS analyzes; Chromatographic condition: Waters BEH C18 chromatographic column, long 50mm, internal diameter 1.0 mm, particle diameter 1.7 μm, column temperature: 40 DEG C; Mobile phase: A phase is 10mM formic acid, B phase is acetonitrile; Flow velocity 0.4mL/min; Mass Spectrometry Conditions: Negative electrospray ionization source ESI-, voltage 2000V, source temp 100 DEG C, taper hole voltage 15V, desolventizing temperature degree 300 DEG C, taper hole gas and desolventizing airshed are respectively 50 and 600L/min; Full scan pattern 50 ~ 1200amu; Secondary collision energy 15V; The intensity of the fragment peak 85 of molecular ion peak 191 is used for the quantitative of glucose 1.4-lactone; Carry out quantitatively with calibration curve method to glucaric acid Isosorbide-5-Nitrae lactone;
4) in Liuwei Dihuang Wan, glucarate and glucaric acid Isosorbide-5-Nitrae lactone detect simultaneously:
Get Liuwei Dihuang Wan, pulverize, precision takes 500mg, add 4.0 mL 60% methanol solutions, ultrasonic 20min, 5,000 leaves heart 10min gets supernatant, residue continues to add 4.0mL 60% methanol solution, ultrasonic 20min, 5000 leave heart 10min gets supernatant, merges supernatant, 14,000 to leave after the heart suitably dilution sample introduction HPLC-LILIC-UV analyzes; HPLC-HILIC-UV method chromatographic condition: chromatographic column is the long 250mm of ZIC-HILIC, internal diameter 4.6mm, granularity 5 μm; With acetonitrile A phase-5mM ammonium dihydrogen phosphate (ADP)+1.0% phosphoric acid B phase for mobile phase, eluent gradient elution program: 0-3min A phase 83%, 3-15min A phase 83-65%, 15-18min A phase 65%, 18-20min A phase 65-83%, 20-30min A phase 83%; Determined wavelength 205nm; Sample introduction 10 μ l, column temperature 30 DEG C; With calibration curve method, simultaneous quantitative is carried out to glucarate and glucaric acid Isosorbide-5-Nitrae lactone.
2. method as claimed in claim 1, is characterized in that described Na
2cO
3solution concentration is 2.0%.
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| US3546205A (en) * | 1967-04-06 | 1970-12-08 | Chugai Pharmaceutical Co Ltd | Stabilizing method and the preparation stabilized thereby |
| CN102590370A (en) * | 2012-01-16 | 2012-07-18 | 南京林业大学 | Method for synchronously determining monosaccharide, uronic acid and saccharic acid in wood fiber material reaction system |
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