CN103543214B - Determination method of content of active ingredient of Pingxiao capsule - Google Patents
Determination method of content of active ingredient of Pingxiao capsule Download PDFInfo
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Abstract
The invention relates to a determination method of the content of an active ingredient of a Pingxiao capsule. The determination method includes preparation of a reference solution, preparation of a test solution and formulation of high performance liquid chromatography conditions, wherein naringin content is not less than 2.13mg/particle and neohesperidin content is not less than 1.22mg/particle. The determination method is simple, safe and reliable, and is capable of faithfully representing product content and quality; the determination method is suitable for industrial daily production and inspection.
Description
Technical field
The present invention relates to field of medicaments, especially relate to the content assaying method of PING XIAO JIAO NANG effective constituent.
Background technology
Existing Chinese patent drug PING XIAO JIAO NANG is a kind of conventional antineoplastic Chinese traditional medicine.[assay] of the PING XIAO JIAO NANG recorded in pharmacopeia and ministerial standard gets this product 30, pour out content, accurately weighed, porphyrize, get powder and be about 4g, accurately weighed, put in 100ml tool plug conical flask, precision adds chloroform 20ml and liquor ammoniae fortis 1ml, close plug, weighed weight, cold soaking 48 hours, or ultrasonic extraction 40 minutes, weigh, the weight of loss is supplied with chloroform, shake well, filter, precision measures filtrate 10ml, put in separating funnel, 4 times are extracted with sulfuric acid solution (0.5mol/L), each 10ml, extract is all filtered in 50ml measuring bottle with the filter paper that sulfuric acid solution (0.5mol/L) is moistening in advance, and with the appropriate washing nozzle of sulfuric acid solution (0.5mol/L), washing lotion is incorporated in measuring bottle, add sulfuric acid solution (0.5mol/L) again to scale, shake up, precision measures 10ml, put in 50ml measuring bottle, add sulfuric acid liquid (0.5mol/L) to scale, shake up according to spectrophotometric method, absorbance log is measured at 262nm and 300nm wavelength place, the heavy this product every of average particle contains vomiting nut in strychnine (C12H22N2O2), should be 0.25 ~ 0.35mg.
PING XIAO JIAO NANG prescription is root tuber of aromatic turmeric 54g hairyvein agrimony 54g excrementum pteropi 45g alum 54g nitre 54g dried lacquer (system) 18g Fructus Aurantii (bran stir-fry) 90g prepared nux vomica 36g, the content of Fructus Aurantii is maximum, it is topmost component, in above-mentioned pharmacopeia, content assaying method only measures the content of strychnine in vomiting nut, truly can not reflect the quality of product, to such an extent as to the stability of product is uncontrollable, bring hidden danger to production and patient.
Summary of the invention
In order to solve the problems of the technologies described above, the invention provides a kind of content assaying method of PING XIAO JIAO NANG effective constituent, the method accurately, reliable, the quality that truly can reflect product.
The present invention is achieved by the following technical solutions:
In PING XIAO JIAO NANG, a content assaying method for effective constituent, comprises the steps:
(1) preparation of reference substance: get aurantiin, neohesperidin reference substance is appropriate;
(2) preparation of test sample: as for subsequent use in volumetric flask after make even capsule for eliminating content methyl alcohol or alcohol extract;
(3) high-efficient liquid phase chromatogram condition: C
184.6 × 250mm, 5 μm of chromatographic columns, mobile phase acetonitrile-water, flow velocity 0.5-1.2mlmin
-1determined wavelength 245-360nm;
(4) determination method: precision is drawn reference substance and need testing solution injection liquid chromatography and be get final product.
Above-mentioned steps (1) described aurantiin reference substance concentration is 80ug/1ml, neohesperidin reference substance concentration 60ug/1ml.
As for for subsequent use in volumetric flask after the ultrasonic extraction of test sample methyl alcohol described in above-mentioned steps (2).Test sample described in preferred steps (2) adds methyl alcohol 25ml, weighed weight, ultrasonic process 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with methyl alcohol, shake up, filter, discard just filtrate, precision measures subsequent filtrate 5ml, put in 25ml measuring bottle, with methanol dilution to scale, shake up, to obtain final product.
In above-mentioned steps (3), the pH value of mobile phase is 2.0-5.0, mobile phase acid for adjusting pH value described in mobile phase acetonitrile-water 15-30: 85-70., is preferably pH value 3.0, mobile phase acetonitrile-water=20: 80; Described acid include but not limited to for phosphoric acid, acetic acid, formic acid, citric acid, tartrate, hydrogen sulfate receive, potassium acid sulfate, hydrochloric acid, sulfuric acid, carbonic acid, perchloric acid, malic acid, citric acid, salicylic acid, caffeic acid etc., preferably phosphoric acid, acetic acid, formic acid, citric acid, tartrate, hydrogen sulfate are received, potassium acid sulfate etc., and the best is phosphoric acid.Described phosphoric acid concentration is 5-20%, and preferred concentration is 10%.In the present invention, preferably 10% phosphoric acid can make each chromatographic peak in PING XIAO JIAO NANG have good separation, improves peak conditions of streaking.
Preferred flow phase acetonitrile-water=20 described in above-mentioned steps (3): 80, flow velocity is 1.0mlmin
-1, determined wavelength 283nm
Measure described in above-mentioned steps (4), preferred naringin content is not less than 2.26mg/ grain, and neohesperidin content is not less than 1.33mg/ grain.
The determination method of content of active ingredient of Pingxiao capsule of the best of the present invention, comprises the steps:
(1) preparation of reference substance: it is appropriate that precision takes aurantiin reference substance, adds methyl alcohol and makes the solution of every 1ml containing aurantiin 80ug; It is appropriate that precision takes neohesperidin reference substance, adds methyl alcohol and make the solution of every 1ml containing neohesperidin 60ug;
(2) get capsule 20, put porphyrize in mortar and cross No. four sieves, get about 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic process 30 minutes, lets cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filter, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methanol dilution to scale, shake up, to obtain final product;
(3) high-efficient liquid phase chromatogram condition
Chromatographic column: WatersC
18post 4.6 × 250mm, 5 μm, mobile phase: acetonitrile-water=20: 80, with 10% phosphoric acid regulating ph value 3.0; Determined wavelength is 283nm; Column temperature: room temperature; Flow velocity: 1.0mlmin
-1; Input mode: auto injection;
(4) determination method is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, to obtain final product.
The prescription of PING XIAO JIAO NANG of the present invention is: weight portion medicinal material root tuber of aromatic turmeric 1-5 part, hairyvein agrimony 1-5 part, excrementum pteropi 1-5 part, alum 1-5, nitre 1-5, dried lacquer 0.5-3 part processed, stir-baked FRUCTUS AURANTII in bran 3-7 part, prepared nux vomica 0.5-4 part.Preferred weight part medicinal material root tuber of aromatic turmeric 2-4 part, hairyvein agrimony 2-4 part, excrementum pteropi 2-4 part, alum 2-4, nitre 2-4 part, dried lacquer 0.5-2 part processed, stir-baked FRUCTUS AURANTII in bran 4-6 part, prepared nux vomica 1-3 part.Optimum weight part medicinal material root tuber of aromatic turmeric 3 parts, hairyvein agrimony 3 parts, excrementum pteropi 2.5 parts, alum 3 parts, 3 parts, nitre, dried lacquer processed 1 part, stir-baked FRUCTUS AURANTII in bran 5 parts, prepared nux vomica 2 parts.
The preparation method of PING XIAO JIAO NANG of the present invention is prepared according to pharmacopeia, preferred following method preparation:
Above 8 taste medicinal materials, get dried lacquer, excrementum pteropi, alum, nitre is ground into fine powder, getting root tuber of aromatic turmeric, stir-baked FRUCTUS AURANTII in bran is pulverized, is that solvent carries out diacolation with ethanol, collects percolate; The dregs of a decoction after diacolation and hairyvein agrimony boiling secondary, filter, collecting decoction; After percolate reclaims ethanol, merge with above-mentioned filtrate, reduced pressure concentration becomes thick paste, dry, pulverize into fine powder, adds prepared nux vomica, above-mentioned fine powder and right amount of auxiliary materials, mixing, granulates, dry, incapsulates, to obtain final product.
Best, preparation method of the present invention, comprises the steps:
Above eight tastes, dried lacquer, excrementum pteropi, alum, nitre are ground into fine powder; Root tuber of aromatic turmeric, stir-baked FRUCTUS AURANTII in bran are ground into most meal, be solvent, carry out diacolation with 70% ethanol, collect percolate; The dregs of a decoction and hairyvein agrimony boiling secondary, filter, collecting decoction; After percolate reclaims ethanol, merge with above-mentioned filtrate, reduced pressure concentration becomes thick paste, dry, pulverize into fine powder, adds prepared nux vomica, above-mentioned fine powder and right amount of auxiliary materials, mixing, granulates, dry, incapsulates, to obtain final product.
In order to better prove the safe and reliable of assay of the present invention, the present invention is verified by following methodology.
Test example Method validation
1 instrument and reagent
Reagent: acetonitrile (chromatographically pure), methyl alcohol, phosphoric acid are analysis alcohol.
Sample: Xi'an Zhengda Pharmaceutical Co., Ltd. provides.
Reference substance: aurantiin reference substance (lot number: 110722-200309), neohesperidin reference substance (lot number: 111857-201001) provide by Nat'l Pharmaceutical & Biological Products Control Institute, for assay.
Instrument: high performance liquid chromatograph (Agilent1200); ; DELTA 320 PH counts (plum Teller-Tuo benefit Instrument Ltd.); AL-204 type electronic analytical balance (Max=210g, d=0.0001g, plum Teller-Tuo benefit Instrument Ltd.); TG332A type micro-analytical balance (Max=20g, d=0.01mg); HQ-500DE type ultrasonic cleaner (Kunshan Ultrasonic Instruments Co., Ltd.).
2, chromatographic condition: see embodiment one
3, reference substance solution preparation: see embodiment one
4, need testing solution preparation: see embodiment one
5, the preparation of the negative need testing solution of Fructus Aurantii is lacked
By prescription composition 1/10th deals, all the other flavour of a drug getting removing Fructus Aurantii together, obtain not containing the negative sample of Fructus Aurantii by technological requirement, get this negative sample, prepare the negative need testing solution of scarce Fructus Aurantii by the preparation method of need testing solution.
6, determination method: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
7, the negative sample interference lacking Fructus Aurantii measures:
The above-mentioned reference substance solution of accurate absorption respectively, the each 10 μ l of negative need testing solution of need testing solution and scarce Fructus Aurantii, injection liquid chromatography, measure, need testing solution has corresponding chromatographic peak existing together mutually to reference substance solution retention time, and the negative need testing solution lacking Fructus Aurantii does not have corresponding chromatographic peak existing together mutually to reference substance solution retention time, but consistent with other chromatographic peak retention time of need testing solution, chromatographic peak abundant information, negative sample is noiseless.
8, the investigation of linear relationship
(concentration is respectively accurate absorption aurantiin reference substance solution respectively, every 1ml is containing aurantiin 8.48ug, 25.44ug, 42.4ug, 59.36ug, 84.8ug) each 10ul, (concentration is respectively neohesperidin reference substance solution, every 1ml is containing neohesperidin 7.95ug, 23.85ug, 39.75ug, 55.65ug, 79.5ug) each 10ul, injection liquid chromatography respectively, measures.With reference substance concentration for horizontal ordinate (X), be that ordinate (Y) carries out linear regression with peak area, obtain aurantiin and neohesperidin equation of linear regression.The aurantiin range of linearity is good linear relationship within the scope of 8.48 ~ 84.8 μ g.Equation of linear regression is Y=15.819X-3.3008; R2=0.9999.Result is respectively in table 1 and Fig. 1.The neohesperidin range of linearity is good linear relationship within the scope of 7.95 ~ 79.5 μ g.Equation of linear regression is Y=17.518X-1.9234; R2=1.Result is respectively in table 2 and Fig. 2.
Table 1 aurantiin linear relationship investigates result
| Sequence number | Aurantiin concentration | Peak area |
| 1 | 8.48μg | 133.2 |
| 2 | 25.44μg | 397.1 |
| 3 | 42.40μg | 671.4 |
| 4 | 59.36μg | 926.8 |
| 5 | 84.80μg | 1342.8 |
Table 2 neohesperidin linear relationship investigates result
| Sequence number | Neohesperidin concentration | Peak area |
| 1 | 7.95μg | 138 |
| 2 | 23.85μg | 418.2 |
| 3 | 39.75μg | 690.8 |
| 4 | 55.65μg | 971.65 |
| 5 | 79.50μg | 1392.75 |
9, precision test
Make even capsule for eliminating need testing solution, by above-mentioned chromatographic condition, repeat sample introduction 6 times respectively, result of calculation, respectively in table 3
Table 3 PING XIAO JIAO NANG precision result
From above result, this instrument precision is good.
10, stability test
At ambient temperature, PING XIAO JIAO NANG need testing solution (110118k criticizes), test sample is prepared by " need testing solution " method, respectively at preparation after 0,2,4,6,8,10,12,14,16,18,20,22, the 24h time interval, aurantiin, neohesperidin content in working sample respectively, and calculate its RSD value.The results are shown in Table 4.
The stability test of table 4 PING XIAO JIAO NANG
Result shows, at room temperature, within 24 hours, internal stability is good for need testing solution.
11, reappearance test
Get the PING XIAO JIAO NANG (110118k criticizes) six parts of same lot number respectively, by the preparation method of need testing solution, prepare need testing solution 6 parts, by above-mentioned chromatographic condition, measure respectively, calculate its content.The results are shown in Table 5.
Table 5 PING XIAO JIAO NANG reappearance is tested
Result shows that the method reappearance is good.
12 recovery tests
Accurate 6 parts, PING XIAO JIAO NANG (110118k criticizes) sample taking known content respectively, according to " Chinese Pharmacopoeia " version in 2010 annex X VIII A quality standards in Chinese drugs analytical approach verification guide principle, accurately weighed aurantiin reference substance, neohesperidin reference substance are appropriate, put in 200ml volumetric flask, add methyl alcohol and dissolve and be settled to scale.Certain density aurantiin reference substance solution (0.2727mg/ml) 10ml of accurate absorption respectively, add in accurately weighed sample, rise from " putting tool plug conical flask; precision adds methyl alcohol 10ml ", to " precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methanol dilution to scale; shake up, to obtain final product." prepare need testing solution.Certain density neohesperidin reference substance solution (0.1568mg/ml) 10ml of accurate absorption adds in accurately weighed sample again, rise from " putting tool plug conical flask; precision adds methyl alcohol 10ml ", to " precision measures subsequent filtrate 5ml; put in 25ml measuring bottle; with methanol dilution to scale, shake up, to obtain final product." prepare need testing solution.The method worked out by text measures content, and with the following formulae discovery recovery, result is respectively in table 6, table 7.
Computing formula:
Reference substance addition (mg)
Table 6 PING XIAO JIAO NANG aurantiin average recovery result
Table 7 PING XIAO JIAO NANG neohesperidin average recovery result
From above-mentioned table 6,7 recovery, this method is safe and reliable, truly can reflect product content.
130 batch sample assay results
Get the PING XIAO JIAO NANG sample of ten lot numbers, the content assaying method worked out according to text prepares need testing solution respectively, analyzes, the results are shown in Table 8 by above-mentioned chromatographic condition.
Table 80 batches of PING XIAO JIAO NANG assay results
| Lot number | Naringin content (mg/ grain) | Neohesperidin content (mg/ grain) |
| 1011129 | 2.92 | 1.71 |
| 1011131 | 3.27 | 1.92 |
| 1011133 | 3.26 | 1.91 |
| 1012135 | 3.19 | 1.88 |
| 1012137 | 2.99 | 1.76 |
| 1012140 | 2.99 | 1.76 |
| 1101155k | 3.14 | 1.76 |
| 1101160k | 2.95 | 1.67 |
| 1101161k | 2.72 | 1.47 |
| 1101162k | 2.97 | 1.57 |
| Average content | 3.04 | 1.74 |
According to 10 batches of PING XIAO JIAO NANG assay results and rate of transform influence factor, limit is decided to be:
Aurantiin: 3.04mg/ grain × 70%=2.13mg/ grain,
Neohesperidin: 1.74mg/ grain × 70%=1.22mg/ grain
In sum, the content assaying method of PING XIAO JIAO NANG of the present invention is simple, reliably, and strong operability, suitable daily production testing.Chromatographic peak degree of separation of the present invention is high.Be separated completely, act charitably in peak, without tailed peak and leading peak, undope in each chromatographic peak impurity peaks.
Accompanying drawing explanation
Fig. 1 aurantiin linear relationship chart
Fig. 2 neohesperidin linear relationship chart
Embodiment
Explaining content of the present invention by embodiment below, is not the further restriction to scope.
Embodiment 1
Get weight portion medicinal material root tuber of aromatic turmeric 54 grams, hairyvein agrimony 54 grams, excrementum pteropi 45 grams, alum 54 grams, 54 grams, nitre, dried lacquer processed 18 grams, stir-baked FRUCTUS AURANTII in bran 90 grams, prepared nux vomica 36 grams; Above eight tastes, dried lacquer, excrementum pteropi, alum, nitre are ground into fine powder; Root tuber of aromatic turmeric, stir-baked FRUCTUS AURANTII in bran are ground into most meal, be solvent, carry out diacolation with 70% ethanol, collect percolate 600ml, reclaim ethanol, for subsequent use; The dregs of a decoction and hairyvein agrimony boiling secondary, filter, merging filtrate also merges with above-mentioned percolate, and reduced pressure concentration becomes thick paste, dry, adds prepared nux vomica, above-mentioned fine powder and starch in right amount, mixing, granulates, dry, incapsulates, makes 1000, to obtain final product.
Content assaying method
(1) preparation of reference substance: it is appropriate that precision takes aurantiin reference substance, adds methyl alcohol and makes the solution of every 1ml containing aurantiin 80ug; It is appropriate that precision takes neohesperidin reference substance, adds methyl alcohol and make the solution of every 1ml containing neohesperidin 60ug
(2) get this product 20, put porphyrize in mortar and cross No. four sieves, get about 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic process 30 minutes, lets cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filter, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methanol dilution to scale, shake up, to obtain final product.
(3) high-efficient liquid phase chromatogram condition
Chromatographic column: WatersC
18post 4.6 × 250mm, 5 μm, mobile phase: acetonitrile-water=20: 80, by 10% phosphoric acid adjust ph 3.0; Determined wavelength is 283nm; Column temperature: room temperature; Flow velocity: 1.0mlmin
-1; Input mode: auto injection.
(4) determination method is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, naringin content 3.04mg/ grain, neohesperidin content 1.74mg/ grain.
Embodiment 2
Reference substance solution is prepared according to embodiment 1
Need testing solution: the PING XIAO JIAO NANG of Example 1 20, puts porphyrize in mortar and crosses No. four sieves, get about 0.5g, accurately weighed, put in tool plug conical flask, precision adds ethanol 25ml refluxing extraction process 30 minutes, let cool, filter, reduced pressure concentration is dry, after dissolving with 25ml methyl alcohol, constant volume is in 25ml volumetric flask again, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methanol dilution to scale, shake up, to obtain final product.
Chromatographic condition: WatersC
18post 4.6 × 250mm, 5 μm, mobile phase: acetonitrile-water=15: 85, by 20% phosphoric acid adjust ph 2.0; Determined wavelength is 283nm; Column temperature: room temperature; Flow velocity: 1.2mlmin
-1; Input mode: auto injection.
Determination method is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, naringin content 2.99mg/ grain, neohesperidin content 1.67mg/ grain.
Embodiment 3
Reference substance solution is prepared according to embodiment 1
Need testing solution: the PING XIAO JIAO NANG of Example 1 20, puts porphyrize in mortar and crosses No. four sieves, get about 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic process 40 minutes, lets cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filter, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methanol dilution to scale, shake up, to obtain final product.
Chromatographic condition: WatersC
18post 4.6 × 250mm, 5 μm, mobile phase: acetonitrile-water=30: 70, with 5% phosphoric acid regulating ph value 5.0; Determined wavelength is 283nm; Column temperature: room temperature; Flow velocity: 0.5mlmin
-1; Input mode: auto injection.
Determination method is accurate respectively draws reference substance solution and each 10 μ l of need testing solution, injection liquid chromatography, measures, naringin content 2.99mg/ grain, neohesperidin content 1.76mg/ grain.
Claims (3)
1. the content assaying method of effective constituent in PING XIAO JIAO NANG, is characterized in that, comprise the steps:
(1) preparation of reference substance: get aurantiin, neohesperidin reference substance is appropriate, making aurantiin reference substance concentration is 80ug/ml, neohesperidin reference substance concentration 60ug/ml;
(2) preparation of test sample: capsule for eliminating sample contents of making even test sample adds methyl alcohol 25ml, weighed weight, ultrasonic process 30 minutes, let cool, more weighed weight, the weight of less loss is supplied with methyl alcohol, shake up, filter, discard just filtrate, precision measures subsequent filtrate 5ml, put in 25ml measuring bottle, with methanol dilution to scale, shake up, to obtain final product;
(3) high-efficient liquid phase chromatogram condition: C184.6 × 250mm, 5 μm of chromatographic columns; Mobile phase acetonitrile-water=15-30: 85-70 is 3.0 by 5-20% phosphoric acid adjust ph; Flow velocity 0.5-1.2mlmin-1 determined wavelength 245-360nm;
(4) determination method: precision is drawn reference substance and need testing solution injection liquid chromatography and be get final product.
2. content assaying method as claimed in claim 1, it is characterized in that: mobile phase acetonitrile-water=20 described in step (3): 80, flow velocity is 1.0mlmin
-1, determined wavelength 283nm.
3. content assaying method as claimed in claim 1, its feature exists, and comprises the steps:
(1) preparation of reference substance: it is appropriate that precision takes aurantiin reference substance, adds methyl alcohol and makes the solution of every 1ml containing aurantiin 80ug;
It is appropriate that precision takes neohesperidin reference substance, adds methyl alcohol and make the solution of every 1ml containing neohesperidin 60ug;
(2) preparation of test sample: capsule for eliminating 20 of making even, puts porphyrize in mortar and crosses No. four sieves, get 0.5g, accurately weighed, put in tool plug conical flask, precision adds methyl alcohol 25ml, weighed weight, ultrasonic process 30 minutes, lets cool, more weighed weight, supply the weight of less loss with methyl alcohol, shake up, filter, discard just filtrate, precision measures subsequent filtrate 5ml, puts in 25ml measuring bottle, with methanol dilution to scale, shake up, to obtain final product;
(3) high-efficient liquid phase chromatogram condition chromatographic column: Waters C18 post 4.6 × 250mm, 5 μm, mobile phase of acetonitrile and water=20: 80, with 10% phosphoric acid regulating ph value 3.0; Determined wavelength is 283nm; Column temperature: room temperature; Flow velocity: 1.0mlmin
-1; Input mode: auto injection;
(4) determination method: accurate absorption reference substance solution and each 10 μ l of need testing solution respectively, injection liquid chromatography, measures, to obtain final product.
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