CN107014921B - The efficient liquid phase detection method of naganol - Google Patents
The efficient liquid phase detection method of naganol Download PDFInfo
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- CN107014921B CN107014921B CN201710223903.XA CN201710223903A CN107014921B CN 107014921 B CN107014921 B CN 107014921B CN 201710223903 A CN201710223903 A CN 201710223903A CN 107014921 B CN107014921 B CN 107014921B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
Abstract
The present invention discloses a kind of efficient liquid phase detection method of naganol, and chromatographic column uses reverse phase C18 chromatographic column；Detector uses DAD detector；Mobile phase A is the aqueous solution of ammonium hydroxide, ammonium acetate and two fourth ammonium acetates；Mobile phase B is ammonium acetate and N, 50% acetonitrile/water mixed solution of the own ammonium of N- dimethyl；Using gradient elution.Method of the invention can effectively detect naganol and its related substance, and separating degree R can be up to 1.5 or more, good separating effect；Detection time is short, only needs 3min that efficient liquid phase detection process can be completed, greatly improves detection efficiency, is suitble to high flux screening；Baseline is steady, does not drift about；Solvent can be saved, cost is reduced, safe operation is simple, handles convenient and efficient；For naganol assay, there is good linear relationship, reproducibility is high, and accuracy and accuracy are high, has important research value in terms of bulk pharmaceutical chemicals, quality of the pharmaceutical preparations research and related pharmacokinetics.
Description
Technical field
The present invention relates to Pharmaceutical Analysis technical fields, and in particular to a kind of efficient liquid phase detection method of naganol.
Background technique
Naganol (suramin) also known as Suramin Sodium, suramin etc. are that German Bayer AG company closed in 1961
At a kind of anti-trypanosome class compound, white is mainly used for treating African typanosomiasis nagana and onchocercosis to buff powder.20
There is scholar to find that naganol is able to suppress the related reverse transcriptase activity of tumour virus, naganol is answered the eighties in century
For the treatment of Immune Deficiency Syndrome (AIDS), show that naganol has one to human immunodeficiency virus (HIV)
Fixed inhibiting effect.The cassie sarcoma and non-hodgkin's that discovery patient suffers from simultaneously when treating AIDS patient using naganol are drenched
Bar tumor subsides completely, can block in conjunction with experiment in vitro discovery naganol certain with the closely related growth factor of tumour growth
With the activity of enzyme, the treatment of various malignant tumours can be widely used in using naganol as a kind of anti-tumor drug, as before
Column gland cancer, lung cancer, colon cancer, fibroid etc..In recent years, naganol also takes in the research of prevention and treatment eye proliferative diseases
Obtained biggish progress.Recently, but have naganol treatment liver fibrosis report.
But naganol is temporarily not evolved to clinical use level, reason is that the physical characteristic of naganol makes it
Polar distribution of field poor distribution in vivo generates pharmacokinetics and the relevant problem of toxicity, to need to reduce dosage with limiting toxicity into one
Step improves the tolerance of patient, so that targeting dispensing is reached maximum, the quantitative detection line of this inevitable requirement naganol is relatively low.
There is presently no the reports of the efficient liquid phase method of detection naganol.According to similar compound in the prior art
Efficient liquid phase detection method is detected, and discovery is poor to the separating effect of naganol, and separating degree R can not be examined effectively less than 1
Individual process impurity peaks or related substance peak out, elution base line easily drift about, integral inaccuracy, when being used for quantitative analysis
Accuracy and accuracy it is not high, and detect that time-consuming needs 15min or more.The present invention for detection method in the prior art into
Gone improvement and optimization, compared with method in the prior art, detection method of the invention not only good separating effect, precision and
Accuracy is high, and safe operation is simple, handles convenient and efficient, is suitble to high flux screening and precisely quantitative.This method is to Ursula
Raw material, quality of the pharmaceutical preparations research and related pharmacokinetics quantitative study of natulanar etc. all have important research value.
Summary of the invention
A kind of the technical problem to be solved by the invention is to provide detection times short, good separating effect, accuracy and accurate
Spend the efficient liquid phase detection method of higher naganol.
In order to solve the above technical problems, the efficient liquid phase detection method of naganol provided by the invention, wherein
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is 0.0005~0.0015% ammonium hydroxide, 1~3mM ammonium acetate
With the aqueous solution of 0.15~0.20mM, bis- fourth ammonium acetate (DBAA)；Mobile phase B be 1.5~4.5mM ammonium acetate and 5~15mMN,
50% acetonitrile/water mixed solution of the own ammonium of N- dimethyl (DMHA)；
Using gradient elution, gradient elution program is carried out by following procedure: mobile phase A+Mobile phase B=100%, 0~
0.01min, it is 20% that Mobile phase B, which keeps percent by volume,；0.01~2.10min, Mobile phase B percent by volume are incremented by by 20%
To 80%；2.10~2.11min, Mobile phase B percentage by volume are decremented to 20% by 80%；2.11~3.00min, Mobile phase B
Keeping percentage by volume is 20%.
In a preferred embodiment, mobile phase A is bis- fourth ammonium acetic acid of 0.001% ammonium hydroxide, 2mM ammonium acetate and 0.18mM
The aqueous solution of salt (DBAA)；Mobile phase B is mixed for 50% acetonitrile/water of 3mM ammonium acetate and the 10mM own ammonium of N, N- dimethyl (DMHA)
Close solution；
In a preferred embodiment, column's length 100mm.
In a preferred embodiment, flow velocity is 1.0~2.0ml/min, more preferably 1.4ml/min.
In a preferred embodiment, Detection wavelength is 250~255nm, more preferably 254nm.
In a preferred embodiment, column temperature control is at 35~40 DEG C, and more preferably 40 DEG C.
In a preferred embodiment, sample volume is 2~8 μ l, more preferably 3~5 μ l.
The present invention also provides a kind of efficient liquid phase methods for measuring naganol content, comprising the following steps:
(1) preparation of reference substance solution and test solution: precision weighs appropriate naganol reference substance, uses water for injection
Dissolution dilutes constant volume into multiple reference substance solutions with a certain concentration gradient；Precision weighs appropriate naganol test sample, uses
Simultaneously constant volume obtains test solution for water for injection dissolution；
(2) chromatographic condition:
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is 0.0005~0.0015% ammonium hydroxide, 1~3mM ammonium acetate
With the aqueous solution of 0.15~0.20mM, bis- fourth ammonium acetate (DBAA)；Mobile phase B be 1.5~4.5mM ammonium acetate and 5~
The 50% acetonitrile/water mixed solution of 15mMDMHA；
Using gradient elution, gradient elution program is carried out by following procedure: mobile phase A+Mobile phase B=100%, 0~
0.01min, it is 20% that Mobile phase B, which keeps percent by volume,；0.01~2.10min, Mobile phase B percent by volume are incremented by by 20%
To 80%；2.10~2.11min, Mobile phase B percentage by volume are decremented to 20% by 80%；2.11~3.00min, Mobile phase B
Keeping percentage by volume is 20%；
(3) measuring method:
The multiple reference substance solution and test solution are pressed into described (2) chromatographic condition successively sample introduction, record chromatography
Figure, prepares linear related work curve according to the spectrum data of multiple reference substance solutions and concentration data, substitutes into test sample
Spectrum data calculates and obtains test solution concentration, completes the measurement of naganol content.
In a preferred embodiment, the concentration of reference substance solution is followed successively by 6.25,12.5,25,50,100,200 μ g/
Ml, flow velocity 1.4ml/min.Detection wavelength is 254nm, and column temperature is 40 DEG C, and sample volume is 3~5 μ l.
The beneficial effect of the efficient liquid phase detection method of naganol provided by the invention is:
1. method of the invention can effectively detect naganol and its related substance, and separating degree R can up to 1.5 with
On, good separating effect.
2. method detection time of the invention is short, only needs 3min that efficient liquid phase detection process can be completed, substantially increase
Detection efficiency is suitble to high flux screening.
3. method measurement HPLC map baseline of the invention is steady, do not drift about.
4. method of the invention can save solvent, cost is reduced, safe operation is simple, handles convenient and efficient.
5. method of the invention is used for the assay of naganol, there is good linear relationship, reproducibility is high, accurately
Degree and accuracy are high, have important research valence in terms of bulk pharmaceutical chemicals, quality of the pharmaceutical preparations research and related pharmacokinetics
Value.
Detailed description of the invention
Fig. 1 is the HPLC map one using method measurement naganol test sample of the invention.
Fig. 2 is the HPLC map two using method measurement naganol test sample of the invention.
Fig. 3 is the HPLC map three using method measurement naganol test sample of the invention.
Fig. 4 is the naganol working curve drawn using method of the invention.
Specific embodiment
Present inventor gropes to have obtained a kind of the efficient of naganol by extensive research and a large amount of experiment
Liquid phase detection method, this method provides can efficiently separate naganol and its flow visualizing in relation to substance and gradient are washed
De- program, will can be difficult in the prior art the naganol efficiently separated and its related substance realizes good separating effect,
Separating degree R is up to 1.5 or more.
The efficient liquid phase detection method for the naganol that inventor uses, chromatographic condition are as follows:
Chromatographic column uses reverse phase C18 chromatographic column, such as using octadecylsilane chemically bonded silica as the Waters of filler
XBridge chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is 0.0005~0.0015% ammonium hydroxide, 1~3mM ammonium acetate
With the aqueous solution of 0.15~0.20mM, bis- fourth ammonium acetate (DBAA)；Mobile phase B is 1~4.5mM ammonium acetate and 5~15mMDMHA
50% acetonitrile/water mixed solution；
Using gradient elution, mobile phase A+Mobile phase B=100%, gradient elution program is carried out by following procedure: 0~
0.01min, it is 20% that Mobile phase B, which keeps percent by volume,；0.01~2.10min, Mobile phase B percent by volume are incremented by by 20%
To 80%；2.10~2.11min, Mobile phase B percentage by volume are decremented to 20% by 80%；2.11~3.00min, Mobile phase B
Keeping percentage by volume is 20%；
In a preferred embodiment of the invention, mobile phase A is bis- fourth of 0.001% ammonium hydroxide, 2mM ammonium acetate and 0.18mM
The aqueous solution of ammonium acetate (DBAA)；Mobile phase B is 50% second of 3mM ammonium acetate and the 10mM own ammonium of N, N- dimethyl (DMHA)
Nitrile/water mixed solution.
In a preferred embodiment of the invention, column's length 100mm.
In a preferred embodiment of the invention, flow velocity is 1.0~2.0ml/min, more preferably 1.4ml/min.
In a preferred embodiment of the invention, Detection wavelength is 250~255nm, more preferably 254nm.
In a preferred embodiment of the invention, column temperature is controlled at 35~40 DEG C, and more preferably 40 DEG C.
In a preferred embodiment of the invention, sample volume is 2~8 μ l, more preferably 3~5 μ l.
Clear, complete description is carried out to technical solution of the present invention below in conjunction with specific embodiment, it is clear that described
Embodiment be a part of the embodiments of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, this field
Those of ordinary skill's every other embodiment obtained without making creative work, belongs to guarantor of the present invention
The range of shield.
Experiment condition in the embodiment of the present invention is as follows:
Instrument: high performance liquid chromatograph (LC-20A)
Chromatographic column: Waters XBridge C18 chromatographic column, column length 100mm；
Test solution: precision weighs naganol test sample 10mg, is placed in 10ml volumetric flask, simultaneously with water for injection dissolution
Constant volume obtains test solution；
Flow velocity: 1.4ml/min；
Detection wavelength: 254nm；
Column temperature: 40 DEG C；
Mobile phase: mobile phase A+Mobile phase B=100%；
Gradient elution: 0~0.01min, it is 20% that Mobile phase B, which keeps percent by volume,；0.01~2.10min, Mobile phase B
Percent by volume is incremented to 80% by 20%；2.10~2.11min, Mobile phase B percentage by volume are decremented to 20% by 80%；
2.11~3.00min, it is 20% that Mobile phase B, which keeps percentage by volume,；
Embodiment 1
Mobile phase A is the aqueous solution of bis- fourth ammonium acetate (DBAA) of 0.001% ammonium hydroxide, 2mM ammonium acetate and 0.18mM；Flowing
Phase B is 50% acetonitrile/water mixed solution of 3mM ammonium acetate and the 10mM own ammonium of N, N- dimethyl (DMHA).
It is according to said method lower by sample introduction three times, HPLC map is as shown in Figure 1-3, baseline is steady, and reproducible, 3min can
Whole appearances, naganol retention time are 1.953~1.959min, theoretical cam curve 9219.
Embodiment 2
Mobile phase A is the aqueous solution of bis- fourth ammonium acetate (DBAA) of 0.0005% ammonium hydroxide, 1mM ammonium acetate and 0.15mM；Stream
Dynamic phase B is 50% acetonitrile/water mixed solution of 1.5mM ammonium acetate and the 5mM own ammonium of N, N- dimethyl (DMHA).
Baseline is steady under the method, and naganol retention time is 2.1min or so, and separating degree is 1.6.
Embodiment 3
Mobile phase A is the aqueous solution of bis- fourth ammonium acetate (DBAA) of 0.0015% ammonium hydroxide, 3mM ammonium acetate and 0.20mM；Stream
Dynamic phase B is 50% acetonitrile/water mixed solution of 4.5mM ammonium acetate and the 15mM own ammonium of N, N- dimethyl (DMHA).
Baseline is steady under the method, and naganol retention time is 1.8min or so, and separating degree is 1.5.
The assay of 4 naganol of embodiment
Based on above-mentioned detection method, inventor also provides a kind of efficient liquid phase method for measuring naganol content, presses
Following steps carry out:
(1) preparation of reference substance solution and test solution: precision weighs appropriate naganol reference substance, uses water for injection
It dissolves and constant volume obtains the stock solution of 1mg/ml, it is accurate to draw 50 μ l stock solutions, constant volume is successively diluted with water for injection to be obtained
6.25, the reference substance solution of 12.5,25,50,100,200ug/ml；Precision weighs appropriate naganol test sample, uses injection
Simultaneously constant volume obtains test solution for water dissolution；
(2) chromatographic condition:
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A is bis- fourth of 0.001% ammonium hydroxide, 2mM ammonium acetate and 0.18mM
The aqueous solution of ammonium acetate (DBAA)；Mobile phase B is 50% second of 3mM ammonium acetate and the 10mM own ammonium of N, N- dimethyl (DMHA)
Nitrile/water mixed solution.
Using gradient elution, gradient elution program carries out 0~0.01min by following procedure, and Mobile phase B keeps volume basis
Than being 20%；0.01~2.10min, Mobile phase B percent by volume are incremented to 80% by 20%；2.10~2.11min, mobile phase
B percentage by volume is decremented to 20% by 80%；2.11~3.00min, it is 20% that Mobile phase B, which keeps percentage by volume,；
(3) measuring method:
6 reference substance solutions and test solution are pressed into the chromatographic condition successively sample introduction, record chromatogram, according to
The naganol peak area and concentration data of 6 reference substance solutions prepare linear related work curve (as shown in Figure 4), the work
Curve linear relationship is good, r >=0.9999；It substitutes into the naganol calculated by peak area of test sample and show that test solution is dense
Extension rate when the test solution concentration and sample introduction of degree, the test solution concentration of comparative measurements and constant volume, calculates
The content of naganol out.
The efficient liquid phase detection method of naganol of the invention can effectively detect naganol and its related substance,
And separating degree R can fill up the vacancy that current naganol content measuring analysis method there is no up to 1.5 or more；Of the invention
The HPLC of detection method composes baseline stability, does not drift about；Method detection time of the invention is short, only needs 3min that height can be completed
Liquid phase detection process is imitated, detection efficiency is substantially increased, is suitble to high flux screening；Method of the invention can save solvent, reduce
Cost, safe operation is simple, handles convenient and efficient；Method of the invention is used for the assay of naganol, has good
Linear relationship, r >=0.9999, reproducibility is high, and accuracy and accuracy are high, in bulk pharmaceutical chemicals, quality of the pharmaceutical preparations research and Related Drug
It is dynamic to learn quantitative study etc. with important research value.
In conclusion the various embodiments described above and attached drawing are only presently preferred embodiments of the present invention, not to limit this
The protection scope of invention, all within the spirits and principles of the present invention, any modification, equivalent substitution, improvement and etc. done all are answered
It is included within the scope of the present invention.
Claims (10)
1. a kind of efficient liquid phase detection method of naganol, which is characterized in that as follows using chromatographic condition:
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A be 0.0005~0.0015% ammonium hydroxide, 1~3mM ammonium acetate and
The aqueous solution of 0.15~0.20mM, bis- fourth ammonium acetate；Mobile phase B is 1.5~4.5mM ammonium acetate and 5~15mM N, N- diformazan
50% acetonitrile/water mixed solution of base hexylamine；
Using gradient elution, gradient elution program is carried out by following procedure: mobile phase A+Mobile phase B=100%, 0~
0.01min, it is 20% that Mobile phase B, which keeps percent by volume,；0.01~2.10min, Mobile phase B percent by volume are incremented by by 20%
To 80%；2.10~2.11min, Mobile phase B percentage by volume are decremented to 20% by 80%；2.11~3.00min, Mobile phase B
Keeping percentage by volume is 20%.
2. the method as described in claim 1, which is characterized in that the mobile phase A be 0.001% ammonium hydroxide, 2mM ammonium acetate and
The aqueous solution of bis- fourth ammonium acetate of 0.18mM；The Mobile phase B is the 50% of 3mM ammonium acetate and 10mM N, N- dimethylhexylamine
Acetonitrile/water mixed solution.
3. the method as described in claim 1, which is characterized in that the column's length is 100mm.
4. the method as described in claim 1, which is characterized in that flow velocity is 1.0~2.0ml/min.
5. the method as described in claim 1, which is characterized in that Detection wavelength is 250~255nm.
6. the method as described in claim 1, which is characterized in that column temperature is controlled at 35~40 DEG C.
7. the method as described in claim 1, which is characterized in that sample volume is 2~8 μ l.
8. a kind of efficient liquid phase method for measuring naganol content, which comprises the following steps:
(1) preparation of reference substance solution and test solution: precision weighs appropriate naganol reference substance, water-soluble with injection
Solution dilutes constant volume into multiple reference substance solutions with a certain concentration gradient；Precision weighs appropriate naganol test sample, with note
It penetrates with water dissolution and constant volume obtains test solution；
(2) chromatographic condition:
Chromatographic column uses reverse phase C18 chromatographic column；
Detector uses DAD detector；
Mobile phase includes mobile phase A and Mobile phase B；Mobile phase A be 0.0005~0.0015% ammonium hydroxide, 1~3mM ammonium acetate and
The aqueous solution of 0.15~0.20mM, bis- fourth ammonium acetate；Mobile phase B is 1.5~4.5mM ammonium acetate and 5~15mM N, N- diformazan
50% acetonitrile/water mixed solution of base hexylamine；
Using gradient elution, gradient elution program is carried out by following procedure: mobile phase A+Mobile phase B=100%, 0~
0.01min, it is 20% that Mobile phase B, which keeps percent by volume,；0.01~2.10min, Mobile phase B percent by volume are incremented by by 20%
To 80%；2.10~2.11min, Mobile phase B percentage by volume are decremented to 20% by 80%；2.11~3.00min, Mobile phase B
Keeping percentage by volume is 20%；
(3) measuring method:
The multiple reference substance solution and test solution are pressed into described (2) chromatographic condition successively sample introduction, record chromatogram, root
Linear related work curve is prepared according to the spectrum data and concentration data of multiple reference substance solutions, substitutes into the map number of test sample
According to calculating and obtaining test solution concentration, the measurement of naganol content is completed.
9. method according to claim 8, which is characterized in that the concentration of reference substance solution is followed successively by 6.25,12.5,25,50,
100、200μg/ml。
10. method according to claim 8, which is characterized in that flow velocity is 1.4ml/min in chromatographic condition, and Detection wavelength is
254nm, column temperature are 40 DEG C, and sample volume is 3~5 μ l.
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746197A (en) * | 2011-04-19 | 2012-10-24 | 亚宝药业集团股份有限公司 | Preparation method of suramin sodium |
| WO2015177329A1 (en) * | 2014-05-23 | 2015-11-26 | INSERM (Institut National de la Santé et de la Recherche Médicale) | Methods for determining whether a patient will achieve a response after radiation therapy |
-
2017
- 2017-04-07 CN CN201710223903.XA patent/CN107014921B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102746197A (en) * | 2011-04-19 | 2012-10-24 | 亚宝药业集团股份有限公司 | Preparation method of suramin sodium |
| WO2015177329A1 (en) * | 2014-05-23 | 2015-11-26 | INSERM (Institut National de la Santé et de la Recherche Médicale) | Methods for determining whether a patient will achieve a response after radiation therapy |
Non-Patent Citations (4)
| Title |
|---|
| Analysis of suramin plasma levels by ion-pair high-performance liquid chromatography under isocratic conditions;RUTH M.RUPRECHT 等;《Journal of Chromatography》;19861231;第378卷;第498-502页 |
| Clinical Pharmacokinetics of Suramin in Patients With HTLV-III/LAV Infection;Jerry M.Collins PhD 等;《J CIIn Pharmacol》;19861231;第26卷;第22-26页 |
| Degradation of suramin in aqueous solutions;J.J. Kettenes-van den Bosch 等;《International Journal of Pharmaceutics》;19970912;第155卷(第1期);第27-34页 |
| Determination of Suramin in Plasma and Urine by Ion-Paired Reverse-Phase High-Performance Liquid Chromatography;Thomas J.Stolzer 等;《Journal of Liquid Chromatography》;19871231;第10卷(第15期);第3451-3462页 |
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