CN106885860A - A kind of method that ASE HPLC methods determine spinosin content in spina date seed - Google Patents
A kind of method that ASE HPLC methods determine spinosin content in spina date seed Download PDFInfo
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- CN106885860A CN106885860A CN201710232354.2A CN201710232354A CN106885860A CN 106885860 A CN106885860 A CN 106885860A CN 201710232354 A CN201710232354 A CN 201710232354A CN 106885860 A CN106885860 A CN 106885860A
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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
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
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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
- G01N2030/062—Preparation extracting sample from raw material
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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
- G01N30/88—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86
- G01N2030/8809—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample
- G01N2030/884—Integrated analysis systems specially adapted therefor, not covered by a single one of the groups G01N30/04 - G01N30/86 analysis specially adapted for the sample organic compounds
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Abstract
The invention discloses a kind of method that ASE HPLC methods determine spinosin content in spina date seed, belong to field of chemical detection.Aim to provide a kind of method that time-consuming ASE extractions that are short and can reach ideal effect are combined with HPLC detection methods.The method is extracted using ASE methods to Spine Date Seed, wherein described ASE methods include first using n-hexane, again with methanol extraction, and and collect methanol extraction liquid；Using HPLC methods to the spinosin content in methanol extraction liquid.The present invention can replace official method to the assay of spinosin in spina date seed, and the content monitoring to the spinosin in spina date seed.
Description
Technical field
The invention belongs to spinosin content in field of chemical detection, especially a kind of ASE-HPLC methods measure spina date seed
Method.
Background technology
《Chinese Pharmacopoeia》Version one prepares test sample method to take this product powder (crossing No. four sieves) about 1g within 2015, and precision claims
Fixed, in putting apparatus,Soxhlet's, plus petroleum ether (60~90 DEG C) is appropriate, is heated to reflux 4 hours, discards petroleum ether liquid, and the dregs of a decoction are flung to
Solvent, is transferred in conical flask, adds 70% ethanol 20ml, is heated to reflux 2 hours, filters, and filter residue is washed with 70% ethanol 5ml
Wash, merge washing lotion and filtrate, to doing, residue adds methyl alcohol to dissolve to recycling design, is transferred in 5ml measuring bottles, plus methyl alcohol is to scale, shakes
Even, filtration takes subsequent filtrate, obtains final product.
The method return time is long, and the professional standards requirement to technical staff is higher.
The content of the invention
For above-mentioned deficiency, the present invention is intended to provide a kind of ASE-HPLC methods that are time-consuming short and can reaching effect same are determined
The method of spinosin content in spina date seed.
In order to solve the above-mentioned technical problem, the technical scheme that the present invention is provided is such：A kind of ASE-HPLC methods are determined
The method of spinosin content, comprises the steps successively in spina date seed：
Step 1：Spine Date Seed is extracted using ASE methods, wherein described ASE methods include first using n-hexane, then
With methanol extraction, and collect methanol extraction liquid；
Step 2：Using HPLC methods to the spinosin content in methanol extraction liquid.
Preferably, described step 1 includes following sub-steps：
Step S1：Spina date seed sample comminution, sieving are taken 1g and be well mixed with 1g diatomite；
Step S2：By the mixture of step 1 gained loaded on being placed with the 10ml ASE abstraction pools of filter membrane, plus diatomite to
Pond mouthful is parallel；
Step S3：With 25ml n-hexane extraction removal of impurities, then 25ml methanol extractions are used, with methanol constant volume to 50ml.
Preferably, the parameter of the removal step described in step S3 is：Temperature is 80 DEG C, and the time is 8min, and number of times is 1 time,
Flush volume is 60%, and purge time is 60s.
Preferably, the parameter of the extraction step described in step S3 is：Temperature is 100 DEG C, and the time is 8min, and number of times is 1 time,
Flush volume is 60%, and purge time is 60s.
Preferably, the detection parameter of the HPLC methods described in step 1 is：Chromatographic column is Thermo AQ；Column temperature is 40 DEG C；Stream
Speed is 0.3mL/min；Mobile phase is acetonitrile-water；Detection wavelength is 335nm.
Preferably, the specification of described chromatographic column is 1.7 μm, 50 × 2.1mm.
Preferably, described mobile phase is added using the method for gradient elution, wherein specific parameter is as follows：
Wash-out total time is 30min；
0~10min, the volume ratio of acetonitrile-water is 12~19 in mobile phase：88~81；
10~16min, the volume ratio of acetonitrile-water is 19~20 in mobile phase：81~80；
16~22min, the volume ratio of acetonitrile-water is 20~100 in mobile phase：80~0；
22~30min, the volume ratio of acetonitrile-water is 100 in mobile phase：0.
The present invention compared with conventional method, with advantages below：
1st, the present invention improves the viscosity of temperature reduction solvent, reduces the prevention that solvent enters sample matrices, increased molten
Agent enters the diffusion of sample matrices, reduces the surface tension between solvent and sample matrices, solvent is dissolved the capacity of determinand
Increase；
2nd, because liquid is much larger than solvability of the gas to solute to the solvability of solute, so the boiling of extraction liquids
Point is improved with pressure rise, so that solvent remains at liquid at high temperature under high pressure；
3rd, the present invention is once investigated to the solvent that Accelerate solvent extraction is used, and is had paper to mention and is extracted using 70% ethanol
Spinosin relative amount is higher, and impurity is less, therefore to having carried out solvent investigation using methyl alcohol and 70% ethanol, as a result shows first
Alcohol is consistent with 70% ethanol extraction spinosin content, and impurity peaks are essentially identical, therefore uses methyl alcohol Extraction solvent；
4th, the main influence for investigating extraction times to result of the present invention, with the method for ASE singles extraction to sample in experiment
Repeat to extract three times, each sample liquid, analysis are received respectively as a result, as a result showing that extraction is once almost complete, therefore extraction
Number of times uses 1 time with time-consuming；
5th, the repeatability of ASE extracting methods of the present invention is good.
Brief description of the drawings
Fig. 1 is the chromatogram of spinosin reference substance；
Fig. 2 is the chromatogram using the spinosin obtained by the extraction of ASE methods；
Fig. 3 is the chromatogram using the spinosin obtained by official method extraction；
Fig. 4 is the linear regression graph carried out with the concentration of spinosin reference substance (mg)-peak area.
Specific embodiment
With reference to specific embodiment, claims of the present invention is described in further detail, but do not constituted
Any limitation of the invention, any limited number of time modification made in the claims in the present invention protection domain, people is in the present invention
Claims within.
Embodiment 1
1st, instrument and equipment and reagent
1.1 instruments：Electronic analytical balance (XA205DU), ASE350 Accelerate solvent extractions instrument (DIONEX companies of the U.S.),
Thermo U3000UHPLC liquid chromatographs.
1.2 reagents：
Water：Meet the one-level water of the regulations of GB/T 6682；
Acetonitrile：Chromatographically pure；
N-hexane, methyl alcohol：Analysis is pure.
2nd, method
The preparation of 2.1 reference substance solutions：
Take spinosin reference substance appropriate, it is accurately weighed, plus methyl alcohol is made solution of every 1ml containing 0.2mg, obtains final product.
The preparation of 2.2 need testing solutions
2.2.1《Chinese Pharmacopoeia》Version one prepares test sample method within 2015：
This product powder (cross No. four sieve) about 1g is taken, accurately weighed, in putting apparatus,Soxhlet's, plus (60~90 DEG C) of petroleum ether is fitted
Amount, is heated to reflux 4 hours, discards petroleum ether liquid, and the dregs of a decoction fling to solvent, are transferred in conical flask, adds 70% ethanol 20ml, plus
Heat backflow 2 hours, filtration, filter residue is washed with 70% ethanol 5ml, merges washing lotion and filtrate, and to doing, residue adds methyl alcohol to recycling design
Dissolving, is transferred in 5ml measuring bottles, plus methyl alcohol is to scale, shakes up, filtration, takes subsequent filtrate, obtains final product.
2.2.2 Accelerate solvent extraction method (ASE) prepares test sample method：
Step S1：Spina date seed sample comminution, sieving are taken 1g and be well mixed with 1g diatomite；
Step S2：By the mixture of step 1 gained loaded on being placed with the 10ml ASE abstraction pools of filter membrane, plus diatomite to
Pond mouthful is parallel；
Step S3：With 25ml n-hexane extraction removal of impurities, then 25ml methanol extractions are used, with methanol constant volume to 50ml.
2.3ASE extraction conditions
The parameter of described removal step is：Temperature is 80 DEG C, and the time is 8min, and number of times is 1 time, and flush volume is
60%, purge time is 60s；
The parameter of described extraction step is：Temperature is 100 DEG C, and the time is 8min, and number of times is 1 time, and flush volume is
60%, purge time is 60s.
2.4 chromatographic conditions and system suitability
With octadecylsilane chemically bonded silica as filler；With octadecylsilane chemically bonded silica as filler.
The detection parameter of HPLC methods is：Chromatographic column is Thermo AQ, 1.7 μm, 50 × 2.1mm；Column temperature is 40 DEG C；Flow velocity
It is 0.3mL/min；Mobile phase is acetonitrile-water；Detection wavelength is 335nm.
Preferably, described mobile phase is added using the method for gradient elution, wherein specific parameter is as follows：
Wash-out total time is 30min；
0~10min, the volume ratio of acetonitrile-water is 12~19 in mobile phase：88~81；
10~16min, the volume ratio of acetonitrile-water is 19~20 in mobile phase：81~80；
16~22min, the volume ratio of acetonitrile-water is 20~100 in mobile phase：80~0；
22~30min, the volume ratio of acetonitrile-water is 100 in mobile phase：0.
2.5 determination methods
Determined according to high performance liquid chromatography (general rule 0512)；
It is accurate respectively to draw reference substance solution and each 10 μ l of need testing solution, liquid chromatograph is injected, determine, obtain final product.
The requirement of 2.6 standard limited values
This product is calculated by dry product, containing spinosin (C28H32O15) 0.080% must not be less than.
2.7 calculate (external standard method)
In formula：CR-reference substance solution concentration, unit is micro- gram per liter (mg/L)；The peak area of AX-test sample；AR—
Reference substance peak area.
Note：
Should be dismantled using preceding extraction bottom of pond portion and cleaned out, otherwise easily cause pressure instability；
The filter paper of abstraction pool bottom should otherwise cause seepage in sealing ring；
Elastic moderate during abstraction pool dress sample, too loose to be easily caused extract solution excessive；
Check whether gas cylinder air pressure reaches 1Mpa before start；
Using being cleaned out after terminating, abstraction pool will dry (get rusty easily) in time.
3rd, result
3.1 linear relationships
Step SS1：Spinosin reference substance is taken, it is accurately weighed, plus methyl alcohol is made solution of every 1ml containing about 0.2mg, i.e.,
；
Step SS2：Then the accurate solution 0.1 μ l, 0.5 μ l, 1 μ l, 1.5 μ l, the 2 μ l of drawing are determined into HPLC respectively,
And determined according to the above method, the results detailed in Table 1；
Step SS3：Linear regression is carried out with concentration (mg)-peak area, Fig. 4 is referred to；
Step SS4：Try to achieve regression equation：Y=6685.2191x-7.7407, R2=0.9999, i.e. spinosin exist
It is in good linear relationship in the range of 0.01439~0.2878mg.
The linear test result of the spinosin of table 1
3.2 replica tests
Take the sample (lot number of identical lot number：1508015) 1g, it is totally 4 parts, accurately weighed, carried by above-mentioned ASE extracting methods
Need testing solution is taken, sample size is 1 μ L, and with above-mentioned chromatographic condition parallel laboratory test, the content for measuring spinosin in sample is shown in
Table 2, RSD is 0.8%, as a result shows that ASE extracting methods repeatability is good.
Table 2 measures the content of spinosin in sample
3.3 precision and stability test
Spinosin reference substance solution (0.1439mg/ml) is taken, continuous sample introduction 6 times records peak area, and peak area RSD is
0.7%, show that instrument precision is good.
Same need testing solution is taken, is placed at room temperature, determined in accordance with the law respectively at 0,2,4,8,12h, refer to Fig. 1.
The RSD of result display spinosin peak area is 0.8%, shows need testing solution stabilization in 12h.
In addition, seeing Fig. 2 using the measure chromatogram of the spinosin in the sample of ASE methods extraction；Carried using official method
The measure chromatogram of the spinosin in the sample for taking is shown in Fig. 3.
3.4 samples difference instrument extract result and with official method results contrast (3 batches)
The sample of table 3 uses the extraction Comparative result of different ASE instrument respectively
The sample of table 4 uses ASE methods and the extraction Comparative result of official method respectively
4 discuss：
The selection of 4.1ASE Extraction solvents：
The present invention is once investigated to the solvent that Accelerate solvent extraction is used, and is had paper to mention and is extracted this using 70% ethanol
Skin promise element relative amount is higher, and impurity is less, therefore to having carried out solvent investigation using methyl alcohol and 70% ethanol, as a result shows methyl alcohol
It is consistent with 70% ethanol extraction spinosin content, and impurity peaks are essentially identical, therefore use methyl alcohol Extraction solvent.
The optimization of 4.2ASE extraction conditions
The main influence for investigating extraction times to result of the invention, with the method for ASE singles extraction to sample weight in experiment
Extract three times again, each sample liquid is received respectively, the results are shown in Table 5, analysis as a result, as a result showing that extraction is once almost complete
Entirely, thus extraction times use 1 time with time-consuming.
Table 5
| Methyl alcohol is extracted | As a result % |
| Extraction 1 time | 0.1311 |
| Extraction 2 times | 0.0002 |
| Extraction 3 times | 0.0008 |
It is above-described be only presently preferred embodiments of the present invention, it is all made in the range of the spirit and principles in the present invention appoint
What modification, equivalent and improvement etc., should be included within the scope of the present invention.
Claims (7)
1. a kind of method that ASE-HPLC methods determine spinosin content in spina date seed, it is characterised in that, successively including following steps
Suddenly:
Step 1:Spine Date Seed is extracted using ASE methods, wherein described ASE methods include first using n-hexane, then uses first
Alcohol is extracted, and collects methanol extraction liquid；
Step 2：Using HPLC methods to the spinosin content in methanol extraction liquid.
2. the method that a kind of ASE-HPLC methods according to claim 1 determine spinosin content in spina date seed, its feature
It is that described step 1 includes following sub-steps：
Step S1：Spina date seed sample comminution, sieving are taken 1g and be well mixed with 1g diatomite；
Step S2：By the mixture of step 1 gained loaded on being placed with the 10ml ASE abstraction pools of filter membrane, plus diatomite to and Chi Kou
It is parallel；
Step S3：With 25ml n-hexane extraction removal of impurities, then 25ml methanol extractions are used, with methanol constant volume to 50ml.
3. the method that a kind of ASE-HPLC methods according to claim 2 determine spinosin content in spina date seed, its feature
It is that the parameter of the removal step described in step S3 is：Temperature is 80 DEG C, and the time is 8min, and number of times is 1 time, and flush volume is
60%, purge time is 60s.
4. the method that a kind of ASE-HPLC methods according to claim 2 determine spinosin content in spina date seed, its feature
It is that the parameter of the extraction step described in step S3 is：Temperature is 100 DEG C, and the time is 8min, and number of times is 1 time, and flush volume is
60%, purge time is 60s.
5. the method that a kind of ASE-HPLC methods according to claim 1 determine spinosin content in spina date seed, its feature
It is that the detection parameter of the HPLC methods described in step 1 is：Chromatographic column is Thermo AQ；Column temperature is 40 DEG C；Flow velocity is 0.3mL/
min；Mobile phase is acetonitrile-water；Detection wavelength is 335nm.
6. the method that a kind of ASE-HPLC methods according to claim 5 determine spinosin content in spina date seed, its feature
It is that the specification of described chromatographic column is 1.7 μm, 50 × 2.1mm.
7. the method that a kind of ASE-HPLC methods according to claim 5 determine spinosin content in spina date seed, its feature
It is that described mobile phase is added using the method for gradient elution, wherein specific parameter is as follows：
Wash-out total time is 30min；
0~10min, the volume ratio of acetonitrile-water is 12~19 in mobile phase：88~81；
10~16min, the volume ratio of acetonitrile-water is 19~20 in mobile phase：81~80；
16~22min, the volume ratio of acetonitrile-water is 20~100 in mobile phase：80~0；
22~30min, the volume ratio of acetonitrile-water is 100 in mobile phase：0.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108181400A (en) * | 2018-01-25 | 2018-06-19 | 南京中医药大学 | The method that UHPLC-QQQ-MS/MS measures 6 kinds of chemical composition contents in spina date seed decocting liquid simultaneously |
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Application publication date: 20170623 |