CN102608250A - Rapid detection method for Jinfangganmao granules - Google Patents
Rapid detection method for Jinfangganmao granules Download PDFInfo
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- CN102608250A CN102608250A CN2012100634309A CN201210063430A CN102608250A CN 102608250 A CN102608250 A CN 102608250A CN 2012100634309 A CN2012100634309 A CN 2012100634309A CN 201210063430 A CN201210063430 A CN 201210063430A CN 102608250 A CN102608250 A CN 102608250A
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Abstract
The invention relates to a rapid detection method for Jinfangganmao granules. The rapid detection method for the Jinfangganmao granules is characterized in that: the identification on paracetamol, ledebouriella root and chlorogenic acid is realized on two thin-layer plates by adopting a thin-layer chromatography (TLC) and using the same testing solution; the fluorescent identification on the ledebouriella root is reported for the first time; the ordinary isocratic elution is adopted, a mixture of acetonitrile, carbinol and 0.1% phosphoric acid which are in a volume ratio of (5.5-6.5):(5-4.5):(90-89.5) is taken as a mobile phase, and the contents of the paracetamol and the chlorogenic acid in a sample are simultaneously determined at the position of 295+/-1 nm, so that the determined indicators which are originally finished through twice quantitative determination can be finished by using once quantitative determination; and the quantitative chromatograms of the two ingredients are excellent in crest separation, the crest retention time for the paracetamol is about 7 minutes, and the crest retention time for the chlorogenic acid is about 15 minutes. The rapid detection method has the advantages of simplicity, convenience, rapidness, accuracy, repeatability and easiness in popularization and grasping, the detection efficiency is effectively increased, the detection cost is lowered, and the environmental pollution is reduced.
Description
Technical field
The present invention relates to the method for quick of the anti-cold granules of a kind of gold.
Background technology
The anti-cold granules (Sugarless type) of gold is for there being sugared type change drug specifications kind, and former specification is every bag of 15g, one time one bag, 3 times on the one, change into after the Sugarless type, every bag of 5g, one time one bag, 3 times on the one.The crude drug amount of taking of every day is constant, but taking dose reduces significantly, and is applicable to diabetic to take.The gold of Sugarless type anti-cold granules prescription composition and method for making are following:
The windproof 233.1g hawthorn of [prescription] Flos Lonicerae 233.1g 233.1g ginger 233.1g paracetamol 56.1g
[method for making] above five kinds of Chinese medicine is got Flos Lonicerae, windproof, hawthorn, adds 8 times of water gagings and decocts secondary, each 1.5 hours; Collecting decoction filters, and filtrating is concentrated into the clear cream that relative density is 1.05～1.10 (50 ℃); Put coldly, add ethanol and make and contain alcohol amount and reach 60%, stir; Left standstill 24 hours, and filtered, filtrate recycling ethanol also is concentrated into the thick paste that relative density is 1.30～1.35 (50 ℃); Ginger is thinly sliced, and adds 5 times of amount alcohol dipping three times, and each 24 hours, merge maceration extract, filter, decompression filtrate recycling ethanol also is concentrated into the thick paste that relative density is 1.30～1.35 (50 ℃); Get paracetamol, mode of progressively increasing with equivalent and Steviosin 18g, dextrin 780g～800g after mixing, add above-mentioned thick paste, stir, and use alcohol granulation, and drying is processed 1000g, promptly gets.
Prevent that by the gold of sugared type the cold granules prescription is formed and method for making is following:
The windproof 77.7g hawthorn of [prescription] Flos Lonicerae 77.7g 77.7g ginger 77.7g paracetamol 18.7g
[method for making] above five kinds of Chinese medicine is got Flos Lonicerae, windproof, hawthorn, adds 8 times of water gagings and decocts secondary, each 1.5 hours; Collecting decoction filters, and filtrating is concentrated into the clear cream that relative density is 1.05～1.10 (50 ℃); Put coldly, add ethanol and make and contain alcohol amount and reach 60%, stir; Left standstill 24 hours, and filtered, filtrate recycling ethanol also is concentrated into the thick paste that relative density is 1.30～1.35 (50 ℃); Ginger is thinly sliced, and adds 5 times of amount alcohol dipping three times, and each 24 hours, merge maceration extract, filter, decompression filtrate recycling ethanol also is concentrated into the thick paste that relative density is 1.30～1.35 (50 ℃); Paracetamol adds 83% ethanol and makes dissolving, adds above-mentioned thick paste and sucrose, stirs, and processes particle 1000g, and drying promptly gets.
Original sugared type quality standard is recorded in national standard for traditional Chinese medicines compilation internal medicine lung system (), and standard No. is: WS-11474 (ZD-1474) 2002.Prescription is made up of honeysuckle, windproof, hawthorn, ginger, paracetamol.Chinese Pharmacopoeia Commission in 2011 has carried out the revision of becoming a full member to standard, and in May, 2011 publicity on the net, the honeysuckle revision in will writing out a prescription in the revised draft of becoming a full member is Flos Lonicerae; The determination of chlorogenic acid revision is acetonitrile-water-phosphoric acid (11: 89: 0.04) for determination of chlorogenic acid in the Flos Lonicerae with acetonitrile-water-phosphoric acid (50: 400: 0.2) specification writing in the honeysuckle, other equal no changes.Revised standard number is: WS-11474 (ZD-1474) 2002-2011Z.
That primary standard has been recorded is windproof, the assay of the discriminating of chlorogenic acid thin layer and chlorogenic acid and paracetamol.Differentiating for two needs 2 kinds of need testing solutions, on two blocks of thin layer plates, adopts two kinds of developping agents, launches respectively to accomplish, and the toxic solvents consumption is big, time-consuming length, contaminated environment; The assay of chlorogenic acid and paracetamol, though moving phase is identical, it is different with the diluted sample multiple to detect wavelength, must accomplish by 2 high performance liquid chromatogram.Because under the detection wavelength 326nm of chlorogenic acid, paracetamol does not have the absorption (see figure 1), and under the detection wavelength 244nm of paracetamol, the very little (see figure 2) of the crest of chlorogenic acid.
The method for quick of the anti-cold granules of gold of the present invention is that with windproof fat-soluble discriminating composition, revision be a water soluble ingredient according to operational characteristic, and differentiates through increasing fluorescence first on the basis that original windproof and chlorogenic acid thin layer are differentiated; Increased the discriminating of paracetamol simultaneously; Three discriminatings are accomplished on two blocks of thin layer plates with the ultrasonic sample solution of same methyl alcohol.Paracetamol and windproofly on a thin layer plate, (see Fig. 3,4), chlorogenic acid is (see figure 5) on another piece thin layer plate.Select chlorogenic acid and paracetamol all to have the 295nm (seeing Fig. 6,7,8) of absorption to be the detection wavelength; With chlorogenic acid in the primary standard and the single separately quantitative measurement of paracetamol; Combine quantitative measurement simultaneously, and former moving phase has been carried out reorganization research, it is undesirable to have solved former chromatographic column durability; The crest of part chromatographic column paracetamol coats the impurity peaks problem, has improved the specificity and the accuracy of quantitative measurement.
Summary of the invention
The present invention is directed to the quality determining method of present Chinese medicine; Sample pre-treatments is more loaded down with trivial details, time-consuming, the murder by poisoning solvent load is big; Environmental pollution is serious, and the present situation that detection speed can't be complementary with the big production of mechanization has been invented and adopted the ultrasonic need testing solution of same methyl alcohol and each control medicinal material solution; On 2 blocks of thin layer plates, completion paracetamol, thin layer windproof and chlorogenic acid are differentiated.Three thin layers are differentiated, only need sample 2g, extract solvent 10ml, 10 minutes time.And, paracetamol and chlorogenic acid have been measured simultaneously at 295nm with the mode of isocratic elution.Make the testing index of second metering mensuration completion originally, can enough quantitative measurements accomplish.Reduce cost, practiced thrift the time, improved efficient.The quantitative chromatogram of binary, crest separates good, and the crest retention time of paracetamol is about 7 minutes, and the crest retention time of chlorogenic acid is about 15 minutes.
According to the extraction process characteristics, the present invention has created the thin layer discrimination method that windproof water soluble ingredient increases fluorescence, has widened windproof discriminating scope.
Water-soluble according to paracetamol and chlorogenic acid much larger than fat-soluble character; Contrast through data; With former extraction solvent absolute ethyl alcohol, revision is 70% methyl alcohol, makes chlorogenic acid contents improve about 30%; Measure the real content (seeing table 1) that numerical value is tending towards sample, effectively improved the accuracy of method.
Through methodological study, the chlorogenic acid sample size is good linear relationship at 0.0926～0.926 μ g with peak area, and regression equation is: Y=2931322.4X-5113, γ=0.999999 (seeing table 2, Fig. 9); The paracetamol sample size is good linear relationship at 0.9576～9.576 μ g with peak area, and regression equation is: Y=271998.7X+18054, γ=0.99997 (seeing table 3, Figure 10).Adopt application of sample to reclaim experiment, the result shows: the average recovery rate that paracetamol is measured for 9 times is 99.76%, and RSD is 1.17% (seeing table 4); The average recovery rate that chlorogenic acid is measured for 9 times is 98.97%, and RSD is 1.95% (seeing table 5).Precision (seeing table 6), stability (seeing table 7), repeatability (seeing table 8), specificity (seeing Figure 11,12,13) all meet the methodology requirement with post durability (seeing table 9, Figure 14,15,16) experiment.Quantitative measurement when being applicable in the anti-cold granules of gold paracetamol and chlorogenic acid.
The technical solution adopted for the present invention to solve the technical problems is:
(1) quick thin layer discrimination method
1. get the anti-cold granules 2～4g of gold, add methyl alcohol 5ml, sonicated 10 minutes filters, and filtrating is as need testing solution.Other gets the paracetamol reference substance, adds methyl alcohol and processes the solution that every 1ml contains 5mg, as reference substance solution; Get windproof control medicinal material 0.3g again, add methyl alcohol 3ml, sonicated 10 minutes, supernatant is as control medicinal material solution; Draw each 4～8 μ l of above-mentioned three kinds of solution, put respectively on same silica GF254 thin layer plate, be 10～12: 2～1 with volume ratio: methenyl choloride-ethyl acetate of 4～2: 1～0.5-methyl alcohol-dense ammonia is developping agent; Launch, take out, dry; Put under the ultraviolet lamp 254nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 1～2 minute are put under the ultraviolet lamp 365nm and are inspected again, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical bright blue look fluorescence principal spot;
2. get the chlorogenic acid reference substance, add methyl alcohol and process the solution that every 1ml contains 2mg, as reference substance solution; Need testing solution 2～5 μ l under drawing reference substance solution 5 μ l and differentiating 1. put respectively on same silica gel g thin-layer plate, and be 15～13: 5～3 with volume ratio: the upper solution of butyl acetate-formic acid of 5～3-water is a developping agent; Launch, take out hot blast drying; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show same color fluorescence spot;
(2). chlorogenic acid and paracetamol be method for quantitatively determining simultaneously
A. the test of chromatographic condition and system suitability is a filling agent with the octadecylsilane chemically bonded silica; With volume ratio is 5.5～6.5: 5～4.5: acetonitrile-methyl alcohol of 90～89.5-0.1% phosphoric acid is moving phase; The detection wavelength is 295nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000;
B. reference substance solution preparation is got chlorogenic acid with the paracetamol reference substance is an amount of, the accurate title calmly, and add methyl alcohol and process every 1ml and contain chlorogenic acid 0.02mg, the solution of paracetamol 0.45mg promptly gets;
C. the anti-cold granules 5g of gold is got in the need testing solution preparation, and porphyrize is got 0.2～0.6g, and accurate title is fixed; Put in the tool plug conical flask, precision adds 70% methyl alcohol 25ml, claims to decide weight, with power 250w, frequency 50kHz; Sonicated 10 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get;
D. accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
These article contain Flos Lonicerae with chlorogenic acid C for every bag
16H
18O
9Meter must not be less than 10.0mg; Contain paracetamol C
8H
9NO
2Should be 90.0%～110.0% of labelled amount.
For the anti-preferred determination techniques scheme of cold granules of sucrose free gold be:
(1) quick thin layer discrimination method
1. get the anti-cold granules 2g of sucrose free gold, add methyl alcohol 5ml, sonicated 10 minutes filters, and filtrating is as need testing solution; Other gets the paracetamol reference substance, adds methyl alcohol and processes the solution that every 1ml contains 5mg, as reference substance solution; Get windproof control medicinal material 0.3g again, add methyl alcohol 3ml, sonicated 10 minutes, supernatant is as control medicinal material solution; Draw each 4 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be 10: 2: 4 with volume ratio: methenyl choloride-ethyl acetate of 1-methyl alcohol-dense ammonia is developping agent, launches; Take out, dry, put under the ultraviolet lamp 254nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 1～2 minute are put under the ultraviolet lamp 365nm and are inspected again, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical bright blue look fluorescence principal spot;
2. get the chlorogenic acid reference substance, add methyl alcohol and process the solution that every 1ml contains 2mg, as reference substance solution; Need testing solution 2～5 μ l under drawing reference substance solution 5 μ l and differentiating 1. put respectively on same silica gel g thin-layer plate, are that the upper solution of butyl acetate-formic acid-water of 15: 5: 5 is a developping agent with volume ratio; Launch, take out hot blast drying; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show same color fluorescence spot;
(2). chlorogenic acid and paracetamol be method for quantitatively determining simultaneously
A. the test of chromatographic condition and system suitability is a filling agent with the octadecylsilane chemically bonded silica; With volume ratio is that acetonitrile-methyl alcohol-0.1% phosphoric acid of 5.5: 4.5: 90 is moving phase; The detection wavelength is 295nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000;
B. reference substance solution preparation is got chlorogenic acid with the paracetamol reference substance is an amount of, the accurate title calmly, and add methyl alcohol and process every 1ml and contain chlorogenic acid 0.02mg, the solution of paracetamol 0.45mg promptly gets;
C. the anti-cold granules 5g of sucrose free gold is got in the need testing solution preparation, and porphyrize is got 0.2g, and accurate title is fixed; Put in the tool plug conical flask, precision adds 70% methyl alcohol 25ml, claims to decide weight, with power 250w, frequency 50kHz; Sonicated 10 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get;
D. accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
These article contain Flos Lonicerae with chlorogenic acid C for every bag
16H
18O
9Meter must not be less than 10.0mg; Contain paracetamol C
8H
9NO
2Should be 90.0%～110.0% of labelled amount.
For the anti-preferred determination techniques scheme of cold granules of the gold that contains sucrose be:
(1) quick thin layer discrimination method
1. get the anti-cold granules 4g of the gold that contains sucrose, add methyl alcohol 5ml, sonicated 10 minutes filters, and filtrating is as need testing solution; Other gets the paracetamol reference substance, adds methyl alcohol and processes the solution that every 1ml contains 5mg, as reference substance solution; Get windproof control medicinal material 0.3g again, add methyl alcohol 3ml, sonicated 10 minutes, supernatant is as control medicinal material solution; Draw each 4 μ l of reference substance solution and control medicinal material solution, need testing solution 8 μ l, put in same silica G F respectively
254On the thin layer plate, be 12: 1.5: 4 with volume ratio: methenyl choloride-ethyl acetate of 0.5-methyl alcohol-dense ammonia is developping agent, launches; Take out, dry, put under the ultraviolet lamp 254nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 1～2 minute are put under the ultraviolet lamp 365nm and are inspected again, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical bright blue look fluorescence principal spot;
2. get the chlorogenic acid reference substance, add methyl alcohol and process the solution that every 1ml contains 2mg, as reference substance solution; Need testing solution 2～5 μ l under drawing reference substance solution 5 μ l and differentiating 1. put respectively on same silica gel g thin-layer plate, are that the upper solution of butyl acetate-formic acid-water of 14: 4: 4 is a developping agent with volume ratio; Launch, take out hot blast drying; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show same color fluorescence spot;
(2). chlorogenic acid and paracetamol be method for quantitatively determining simultaneously
A. the test of chromatographic condition and system suitability is a filling agent with the octadecylsilane chemically bonded silica; With volume ratio is that acetonitrile-methyl alcohol-0.1% phosphoric acid of 6: 4.5: 89.5 is moving phase; The detection wavelength is 295nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000;
B. reference substance solution preparation is got chlorogenic acid with the paracetamol reference substance is an amount of, the accurate title calmly, and add methyl alcohol and process every 1ml and contain chlorogenic acid 0.02mg, the solution of paracetamol 0.45mg promptly gets;
C. the anti-cold granules 5g of the gold that contains sucrose is got in the need testing solution preparation, and porphyrize is got 0.6g, and accurate the title decides; Put in the tool plug conical flask, precision adds 70% methyl alcohol 25ml, claims to decide weight, with power 250w, frequency 50kHz; Sonicated 10 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get;
D. accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
These article contain Flos Lonicerae with chlorogenic acid C for every bag
16H
18O
9Meter must not be less than 10.0mg; Contain paracetamol C
8H
9NO
2Should be 90.0%～110.0% of labelled amount.
Principle of the present invention is following:
1. by the performance of methyl alcohol solubilized polarity and nonpolar multiple composition, be to extract solvent, extract the sample and the control medicinal material solution that obtain the perfect information amount with methyl alcohol.According to effective constituent chemical constitution and polarity separately, under specific unfolding condition, utilize its absorption, desorption ability on thin layer plate different again, make each effective constituent be able to separate.The approximate effective constituent of polarity like this, on same block of thin layer plate, different inspects under the condition, can demonstrate the different spot colors of Rf value, detects several compositions without interfering with each other and be used for the while.
2. all present the character of absorption in the ultraviolet region according to chlorogenic acid and paracetamol,, reduce the high paracetamol peak area of content for increasing the chlorogenic acid peak area of low content; Selection chlorogenic acid and paracetamol all have the 295nm of absorption as measuring wavelength; Make the crest area sizableness of chlorogenic acid and paracetamol, and crest area separately, in certain scope; Present good linear relationship with sample size again, and be used for quantitative measurement.Component through moving phase is inquired into ratio again, make chlorogenic acid and paracetamol not only crest separate well, and the crest retention time suits about 7 minutes of the crest retention time of paracetamol, about 15 minutes of the crest retention time of chlorogenic acid.
Innovative point of the present invention and beneficial effect are following:
(1) adopting common isocratic elution, reverse-phase chromatographic column first, is 5.5～6.5: 5～4.5 with volume ratio: acetonitrile-methyl alcohol of 90～89.5-0.1% phosphoric acid is moving phase; At the 295nm place, chlorogenic acid and paracetamol content in the golden anti-cold granules have been measured simultaneously.Make 2 days workload originally, shorten to completion in a day, and practiced thrift moving phase and sample preparation reagent at double.
(2) water-soluble according to paracetamol and chlorogenic acid much larger than fat-soluble character; Contrast through data; Methyl alcohol with 70% replaces absolute ethyl alcohol, and having solved former method can not extract chlorogenic acid fully, causes measuring the problem that numerical value departs from real content; It is about 30% that chlorogenic acid contents is improved, and improved the accuracy of method.
(3) the present invention adopts the means that increase fluorescence first; Windproof water soluble ingredient has been carried out the thin layer fluorescence identification; The discriminating new method of windproof medicinal material water soluble ingredient in the compound preparation not only is provided, and has solved former thin layer identification beacon and water extraction process disconnection, can't bring into play the effect of monitoring.
(4) three thin layers of the present invention are differentiated only needs sample 2g, and sample, control medicinal material and reference substance pre-treatment, and all being that methyl alcohol is ultrasonic gets final product, easy, quick, only needs methyl alcohol 10ml, 10 minutes time.Compare with former binomial discriminating, under the situation that increases a discriminating, also practice thrift solvent 42ml, 1.3 hours time.Make thin layer differentiate the control extraction process effect of having brought into play simultaneously.
(5) appearance of the inventive method, not merely the fast detecting for the anti-cold granules of gold provides method, but also is the content great disparity, detects the different different compounds quantitative measurement simultaneously of wavelength, the research thinking is provided, tool table general and exemplary role.
Description of drawings
The HPLC chromatogram that Fig. 1 detects with the anti-cold granules 326nm of a collection of gold
The HPLC chromatogram that Fig. 2 detects with the anti-cold granules 244nm of a collection of gold
The paracetamol spot of inspecting under Figure 32 54nm
The windproof fluorescence spot that Figure 41 0% sulfuric acid colour developing back 365nm inspects
The chlorogenic acid fluorescence spot that Figure 53 65nm inspects
The spectral scan figure of Fig. 6 paracetamol
The spectral scan figure of Fig. 7 chlorogenic acid
The HPLC chromatogram that Fig. 8 detects with the anti-cold granules 295nm of a collection of gold
The linear relationship chart of Fig. 9 chlorogenic acid
The linear relationship chart of Figure 10 paracetamol
Figure 11 chlorogenic acid and paracetamol reference substance HPLC chromatogram
Figure 12 is the anti-cold granules HPLC chromatogram of gold
Figure 13 is the anti-cold granules HPLC chromatogram of the gold that does not contain paracetamol and Flos Lonicerae
Figure 14 serviceability test-Jin Dao Tianjin, island VP-ODS post (sample HPLC chromatogram of 4.6 * 150mm)
Figure 15 serviceability test-Di Ma dimonsil post (sample HPLC chromatogram of 4.6 * 150mm)
Figure 16 serviceability test-GraceSmart RP post (sample HPLC chromatogram of 4.6 * 250mm)
Among Fig. 1, Fig. 2, Fig. 8, Figure 11, Figure 12, Figure 14, Figure 15, Figure 16,1 is the paracetamol peak, and 2 is the chlorogenic acid peak
Fig. 3, Fig. 4 are same block of thin layer plate, and Fig. 3 is the paracetamol spot of under uviol lamp 254nm, inspecting, after Fig. 4 is the colour developing of 10% ethanol solution of sulfuric acid; The windproof fluorescence spot of under uviol lamp 365nm, inspecting that increases, the sample label of Fig. 3, Fig. 4 is the same, and 1 is windproof control medicinal material; 2 is windproof blank; 3,4,5 is sample, and 6 is paracetamol, and 7 is that paracetamol is blank
Among Fig. 5,1 is chlorogenic acid, and 2 is that blank 3.4.5 is a sample
Among Fig. 9, Figure 10, ordinate is a peak area; Horizontal ordinate is sample size (μ g)
The specific embodiment of the invention
The anti-cold granules method for quick of embodiment 1 sucrose free gold
(1) quick thin layer discrimination method
1. get the anti-cold granules 2g of sucrose free gold, add methyl alcohol 5ml, sonicated 10 minutes filters, and filtrating is as need testing solution; Other gets the paracetamol reference substance, adds methyl alcohol and processes the solution that every 1ml contains 5mg, as reference substance solution; Get windproof control medicinal material 0.3g again, add methyl alcohol 3ml, sonicated 10 minutes, supernatant is as control medicinal material solution; Draw each 4 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be 10: 2: 4 with volume ratio: methenyl choloride-ethyl acetate of 1-methyl alcohol-dense ammonia is developping agent, launches; Take out, dry, put under the ultraviolet lamp 254nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 1～2 minute are put under the ultraviolet lamp 365nm and are inspected again, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical bright blue look fluorescence principal spot;
2. get the chlorogenic acid reference substance, add methyl alcohol and process the solution that every 1ml contains 2mg, as reference substance solution; Need testing solution 2～5 μ l under drawing reference substance solution 5 μ l and differentiating 1. put respectively on same silica gel g thin-layer plate, are that the upper solution of butyl acetate-formic acid-water of 15: 5: 5 is a developping agent with volume ratio; Launch, take out hot blast drying; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show same color fluorescence spot;
(2). chlorogenic acid and paracetamol be method for quantitatively determining simultaneously
A. the test of chromatographic condition and system suitability is a filling agent with the octadecylsilane chemically bonded silica; With volume ratio is that acetonitrile-methyl alcohol-0.1% phosphoric acid of 5.5: 4.5: 90 is moving phase; The detection wavelength is 295nm.Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000;
B. reference substance solution preparation is got chlorogenic acid with the paracetamol reference substance is an amount of, the accurate title calmly, and add methyl alcohol and process every 1ml and contain chlorogenic acid 0.02mg, the solution of paracetamol 0.45mg promptly gets;
C. the anti-cold granules 5g of sucrose free gold is got in the need testing solution preparation, and porphyrize is got 0.2g, and accurate title is fixed; Put in the tool plug conical flask, precision adds 70% methyl alcohol 25ml, claims to decide weight, with power 250w, frequency 50kHz; Sonicated 10 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get;
D. accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
These article contain Flos Lonicerae with chlorogenic acid C for every bag
16H
18O
9Meter must not be less than 10.0mg; Contain paracetamol C
8H
9NO
2Should be 90.0%～110.0% of labelled amount.The mensuration result of three lot sample article sees table 10.
(1) quick thin layer discrimination method
1. get the anti-cold granules 4g of the gold that contains sucrose, add methyl alcohol 5ml, sonicated 10 minutes filters, and filtrating is as need testing solution; Other gets the paracetamol reference substance, adds methyl alcohol and processes the solution that every 1ml contains 5mg, as reference substance solution; Get windproof control medicinal material 0.3g again, add methyl alcohol 3ml, sonicated 10 minutes, supernatant is as control medicinal material solution; Draw each 4 μ l of reference substance solution and control medicinal material solution, need testing solution 8 μ l, put in same silica G F respectively
254On the thin layer plate, be 12: 1.5: 4 with volume ratio: methenyl choloride-ethyl acetate of 0.5-methyl alcohol-dense ammonia is developping agent, launches; Take out, dry, put under the ultraviolet lamp 254nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 1～2 minute are put under the ultraviolet lamp 365nm and are inspected again, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical bright blue look fluorescence principal spot;
2. get the chlorogenic acid reference substance, add methyl alcohol and process the solution that every 1ml contains 2mg, as reference substance solution; Need testing solution 2～5 μ l under drawing reference substance solution 5 μ l and differentiating 1. put respectively on same silica gel g thin-layer plate, are that the upper solution of butyl acetate-formic acid-water of 14: 4: 4 is a developping agent with volume ratio; Launch, take out hot blast drying; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show same color fluorescence spot;
(2). chlorogenic acid and paracetamol be method for quantitatively determining simultaneously
A. the test of chromatographic condition and system suitability is a filling agent with the octadecylsilane chemically bonded silica; With volume ratio is that acetonitrile-methyl alcohol-0.1% phosphoric acid of 6: 4.5: 89.5 is moving phase; The detection wavelength is 295nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000;
B. reference substance solution preparation is got chlorogenic acid with the paracetamol reference substance is an amount of, the accurate title calmly, and add methyl alcohol and process every 1ml and contain chlorogenic acid 0.02mg, the solution of paracetamol 0.45mg promptly gets;
C. the anti-cold granules 5g of the gold that contains sucrose is got in the need testing solution preparation, and porphyrize is got 0.6g, and accurate the title decides; Put in the tool plug conical flask, precision adds 70% methyl alcohol 25ml, claims to decide weight, with power 250w, frequency 50kHz; Sonicated 10 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get.
D. accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
These article contain Flos Lonicerae with chlorogenic acid C for every bag
16H
18O
9Meter must not be less than 10.0mg; Contain paracetamol C
8H
9NO
2Should be 90.0%～110.0% of labelled amount.The mensuration result of three lot sample article sees table 10.
Different solvent chlorogenic acid and the paracetamol content results (mg/g) extracted of the same lot sample article of table 1
Table 2 chlorogenic acid sample size and peak area
Table 3 paracetamol sample size and peak area
The recovery test result of paracetamol in table 4 sample
The recovery test result of chlorogenic acid in table 5 sample
Annotate: for practicing thrift reference substance, the cumulative volume of sample is not 25ml, is 15ml, and under the consistent situation of concentration, sampling amount reduces.
Table 6 precision experimental result (peak area)
Table 7 stability experiment result
Table 8 replica test result
The content of the same sample that the different chromatographic columns of table 9 are measured
Paracetamol and determination of chlorogenic acid result in the anti-cold granules of table 10 gold
Claims (4)
1. the present invention relates to the method for quick of the anti-cold granules of a kind of gold, it is characterized in that:
(1) quick thin layer discrimination method
1. get the anti-cold granules 2～4g of gold, porphyrize adds methyl alcohol 5ml, and sonicated 10 minutes filters, and filtrating is as need testing solution; Other gets the paracetamol reference substance, adds methyl alcohol and processes the solution that every 1ml contains 5mg, as reference substance solution; Get windproof control medicinal material 0.3g again, add methyl alcohol 3ml, sonicated 10 minutes, supernatant is as control medicinal material solution; Draw each 4～8 μ l of above-mentioned three kinds of solution, put respectively on same silica GF254 thin layer plate, be 10～12: 2～1 with volume ratio: methenyl choloride-ethyl acetate of 4～2: 1～0.5-methyl alcohol-dense ammonia is developping agent; Launch, take out, dry; Put under the ultraviolet lamp 254nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 1～2 minute are put under the ultraviolet lamp 365nm and are inspected again, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical bright blue look fluorescence principal spot;
2. get the chlorogenic acid reference substance, add methyl alcohol and process the solution that every 1ml contains 2mg, as reference substance solution; Need testing solution 2～5 μ l under drawing reference substance solution 5 μ l and differentiating 1. put respectively on same silica gel g thin-layer plate, and be 15～13: 5～3 with volume ratio: the upper solution of butyl acetate-formic acid of 5～3-water is a developping agent; Launch, take out hot blast drying; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show same color fluorescence spot;
(2). chlorogenic acid and paracetamol be method for quantitatively determining simultaneously
A. the test of chromatographic condition and system suitability is a filling agent with the octadecylsilane chemically bonded silica; With volume ratio is 5.5～6.5: 5～4.5: acetonitrile-methyl alcohol of 90～89.5-0.1% phosphoric acid is moving phase; The detection wavelength is 295nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000;
B. reference substance solution preparation is got chlorogenic acid with the paracetamol reference substance is an amount of, the accurate title calmly, and add methyl alcohol and process every 1ml and contain chlorogenic acid 0.02mg, the solution of paracetamol 0.45mg promptly gets;
C. the anti-cold granules 5g of gold is got in the need testing solution preparation, and porphyrize is got 0.2～0.6g, and accurate title is fixed; Put in the tool plug conical flask, precision adds 70% methyl alcohol 25ml, claims to decide weight, with power 250w, frequency 50kHz; Sonicated 10 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get;
D. accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
These article contain Flos Lonicerae with chlorogenic acid C for every bag
16H
18O
9Meter must not be less than 10.0mg; Contain paracetamol C
8H
9NO
2Should be 90.0%～110.0% of labelled amount.
2. the method for quick of the anti-cold granules of a kind of gold according to claim 1 is characterized in that the anti-cold granules of described gold is meant that anti-cold granules of the gold that contains sucrose and sucrose free gold prevent two kinds of cold granules.
3. according to the method for quick of the anti-cold granules of the described a kind of gold of claim 1-2, its characteristic also is:
(1) quick thin layer discrimination method
1. get the anti-cold granules 2g of sucrose free gold, porphyrize adds methyl alcohol 5ml, and sonicated 10 minutes filters, and filtrating is as need testing solution; Other gets the paracetamol reference substance, adds methyl alcohol and processes the solution that every 1ml contains 5mg, as reference substance solution; Get windproof control medicinal material 0.3g again, add methyl alcohol 3ml, sonicated 10 minutes, supernatant is as control medicinal material solution; Draw each 4 μ l of above-mentioned three kinds of solution, put in same silica G F respectively
254On the thin layer plate, be 10: 2: 4 with volume ratio: methenyl choloride-ethyl acetate of 1-methyl alcohol-dense ammonia is developping agent, launches; Take out, dry, put under the ultraviolet lamp 254nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 1～2 minute are put under the ultraviolet lamp 365nm and are inspected again, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical bright blue look fluorescence principal spot;
2. get the chlorogenic acid reference substance, add methyl alcohol and process the solution that every 1ml contains 2mg, as reference substance solution; Need testing solution 2～5 μ l under drawing reference substance solution 5 μ l and differentiating 1. put respectively on same silica gel g thin-layer plate, are that the upper solution of butyl acetate-formic acid-water of 15: 5: 5 is a developping agent with volume ratio; Launch, take out hot blast drying; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show same color fluorescence spot;
(2). chlorogenic acid and paracetamol be method for quantitatively determining simultaneously
A. the test of chromatographic condition and system suitability is a filling agent with the octadecylsilane chemically bonded silica; With volume ratio is that acetonitrile-methyl alcohol-0.1% phosphoric acid of 5.5: 4.5: 90 is moving phase; The detection wavelength is 295nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000;
B. reference substance solution preparation is got chlorogenic acid with the paracetamol reference substance is an amount of, the accurate title calmly, and add methyl alcohol and process every 1ml and contain chlorogenic acid 0.02mg, the solution of paracetamol 0.45mg promptly gets;
C. the need testing solution preparation is got and is not contained the anti-cold granules 5g of sucrose gold, and porphyrize is got 0.2g, and accurate title is fixed; Put in the tool plug conical flask, precision adds 70% methyl alcohol 25ml, claims to decide weight, with power 250w, frequency 50kHz; Sonicated 10 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get;
D. accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
These article contain Flos Lonicerae with chlorogenic acid C for every bag
16H
18O
9Meter must not be less than 10.0mg; Contain paracetamol C
8H
9NO
2Should be 90.0%～110.0% of labelled amount.
4. according to the method for quick of the anti-cold granules of the described a kind of gold of claim 1-2, its characteristic also is:
(1) quick thin layer discrimination method
1. get the anti-cold granules 4g of the gold that contains sucrose, porphyrize adds methyl alcohol 5ml, and sonicated 10 minutes filters, and filtrating is as need testing solution; Other gets the paracetamol reference substance, adds methyl alcohol and processes the solution that every 1ml contains 5mg, as reference substance solution; Get windproof control medicinal material 0.3g again, add methyl alcohol 3ml, sonicated 10 minutes, supernatant is as control medicinal material solution; Draw each 4 μ l of reference substance solution and control medicinal material solution, need testing solution 8 μ l, put respectively on same silica GF254 thin layer plate, be 12: 1.5: 4 with volume ratio: methenyl choloride-ethyl acetate of 0.5-methyl alcohol-dense ammonia is developping agent; Launch, take out, dry; Put under the ultraviolet lamp 254nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show the same color spot; Spray with 10% ethanol solution of sulfuric acid, 105 ℃ of bakings 1～2 minute are put under the ultraviolet lamp 365nm and are inspected again, in the test sample chromatogram, with the corresponding position of control medicinal material chromatogram on, show identical bright blue look fluorescence principal spot;
2. get the chlorogenic acid reference substance, add methyl alcohol and process the solution that every 1ml contains 2mg, as reference substance solution; Need testing solution 2～5 μ l under drawing reference substance solution 5 μ l and differentiating 1. put respectively on same silica gel g thin-layer plate, are that the upper solution of butyl acetate-formic acid-water of 14: 4: 4 is a developping agent with volume ratio; Launch, take out hot blast drying; Put under the ultraviolet lamp 365nm and inspect; In the test sample chromatogram, with the corresponding position of reference substance chromatogram on, show same color fluorescence spot;
(2). chlorogenic acid and paracetamol be method for quantitatively determining simultaneously
A. the test of chromatographic condition and system suitability is a filling agent with the octadecylsilane chemically bonded silica; With volume ratio is that acetonitrile-methyl alcohol-0.1% phosphoric acid of 6: 4.5: 89.5 is moving phase; The detection wavelength is 295nm; Number of theoretical plate calculates by the chlorogenic acid peak should be not less than 3000;
B. reference substance solution preparation is got chlorogenic acid with the paracetamol reference substance is an amount of, the accurate title calmly, and add methyl alcohol and process every 1ml and contain chlorogenic acid 0.02mg, the solution of paracetamol 0.45mg promptly gets;
C. the anti-cold granules 5g of the gold that contains sucrose is got in the need testing solution preparation, and porphyrize is got 0.6g, and accurate the title decides; Put in the tool plug conical flask, precision adds 70% methyl alcohol 25ml, claims to decide weight, with power 250w, frequency 50kHz; Sonicated 10 minutes is put coldly, claims to decide weight again, supplies the weight that subtracts mistake with 70% methyl alcohol; Shake up, filter, promptly get;
D. accurate respectively reference substance solution and each the 5 μ l of need testing solution of drawing of determination method inject liquid chromatograph, measure, and promptly get;
These article contain Flos Lonicerae with chlorogenic acid C for every bag
16H
18O
9Meter must not be less than 10.0mg; Contain paracetamol C
8H
9NO
2Should be 90.0%～110.0% of labelled amount.
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| CN110455976A (en) * | 2019-08-30 | 2019-11-15 | 广西壮族自治区药用植物园 | A kind of thin-layer chromatography detection method of " radix scutellariae adds taste disinfectant soup " extract |
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| CN110133138A (en) * | 2019-05-22 | 2019-08-16 | 贵州天楼生物发展有限公司 | The detection method of stauntonvine Content of Chlorogenic Acid |
| CN110455976A (en) * | 2019-08-30 | 2019-11-15 | 广西壮族自治区药用植物园 | A kind of thin-layer chromatography detection method of " radix scutellariae adds taste disinfectant soup " extract |
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