CN110672736B - Quality identification and determination method for ginger-processed American ginseng processed product - Google Patents

Quality identification and determination method for ginger-processed American ginseng processed product Download PDF

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CN110672736B
CN110672736B CN201910924382.XA CN201910924382A CN110672736B CN 110672736 B CN110672736 B CN 110672736B CN 201910924382 A CN201910924382 A CN 201910924382A CN 110672736 B CN110672736 B CN 110672736B
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ginsenoside
retention time
relative retention
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ginger
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谢勇
刘忠英
洪梅
袁小平
胡明欣
睢诚
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Jilin Province Beiyuhong Pharmaceutical Co.,Ltd.
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Jilin Beiyu American Ginseng Research Co ltd
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Abstract

The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a quality identification and determination method for a ginger-processed American ginseng processed product, which is characterized by comprising the following steps of: preparation of control solutions: weighing a certain amount of ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rc and ginsenoside Rd, precisely weighing, and adding methanol to prepare a solution containing ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rc and ginsenoside Rd in each 1ml by the mass ratio of 0.06-0.08:0.6-0.75:1-1.2:0.1-0.12: 0.1-0.15; and carrying out the subsequent quality identification and determination steps. The method is accurate, reduces impurity interference, and is efficient and reliable.

Description

Quality identification and determination method for ginger-processed American ginseng processed product
Technical Field
The invention belongs to the technical field of pharmaceutical analysis, and particularly relates to a quality identification and determination method for a ginger-processed American ginseng processed product.
Background
The radix Panacis Quinquefolii is Panax quinquefolium of Panax of Araliaceae, and is native to North America and south Canada. In 1718, the year Yuanda Canada, China, recorded in "materia Medica, New slave, and Bing: bitter, cold and slightly sweet, thick and thin in flavor, tonifying lung to reduce fire, producing body fluid, relieving restlessness and fatigue, and being suitable for patients with fire due to deficiency, which is seen in the Western Fland West. (similar to Rough ginseng in Liaodong, the decocted herb is not fragrant, the smell is very thin, and the pill is contraindicated to be the same as that of the pearl ginseng) (the pill is contraindicated to be taken for patients with cold in the zang-organs, namely, taken as abdominal pain, taken with stagnated fire, not fully developed fire and capable of generating cold and heat). The book of examination of drug properties, Yu: ' American ginseng is similar to Liaoshen's bark diced ginseng, which is similar to ginseng in taste, but cold in nature, sweet and bitter in taste, tonifying yin and reducing fever, ginger processed, tonifying primordial qi and strengthening healthy qi '. The compendium of materia Medica is collected from materia Medica and drug property examination, and the attention on processing that stir-frying with iron fire is forbidden is provided. American ginseng is used in China for only 300 years, most people using the American ginseng are those of official and noble people, the using amount is small, and the American ginseng is successfully introduced and cultivated in the first ginseng field of Ji-Lin province in the early 80 s. Along with the improvement of living standard of people and the mass planting of American ginseng made in China, the price is also reduced, and the American ginseng health-care tea is widely applied to the aspects of improving immunity, resisting fatigue, protecting cardiovascular system, reducing blood sugar, resisting cancer and the like in clinic.
American ginseng also has clinical use contraindications, and the Chinese herbal dictionary and the Chinese herbal medicine are all used for explaining that the patients with cold-dampness in the stomach are prohibited to take the American ginseng, and the patients with cold in the viscera are taken as abdominal pain, stagnated fire, and the fire does not occur thoroughly to generate cold and heat. Therefore, the processing method of American ginseng is largely recorded in Wu Jutong medical records, such as stir-frying ginger juice, stir-frying ginger blocks into yellow, stir-frying ginger juice into yellow, stir-frying ginger slices into dry, stir-frying ginger, and the like, and the record of ginger-processed American ginseng is recorded in Wu Jutong medical records; zhang 32895Qing Yi Bian (a records of medical records of Shanren) and so on, also use "make xi Yang Shen" many times. The significance lies in that the cold and cool nature of American ginseng has the pungent and warm nature of ginger, which can solve the defect of the clinical prohibition of patients with middle-jiao spleen and stomach cold-dampness, and the pungent and dispersing nature of ginger can supplement the qi-tonifying function of American ginseng, so the medicine property examination says 'ginger essence is good for the first and right qi'.
The traditional simple methods such as visual inspection, mouth taste, nasal smell, hand touch and the like are very limited in traditional Chinese medicine identification, but a great number of false positive and false negative problems exist in chromatographic methods such as HPLC, IR, NIR and TLC, and deviation of conclusion is easily caused. The ginger-processed American ginseng is a processed product of American ginseng, the drug properties and functions of the ginger-processed American ginseng have certain differences from those of the American ginseng, and no effective distinguishing method for the quality of the ginger-processed American ginseng exists in the prior art; based on the method, the invention provides a method for distinguishing ginger-processed American ginseng efficiently and accurately.
Disclosure of Invention
In order to solve the technical problems, the invention provides a method for identifying and measuring the quality of a processed ginger American ginseng product, which has a precise measurement area, reduces impurity interference, and is efficient and reliable.
The technical scheme of the invention is as follows:
a quality identification and determination method for a ginger-processed American ginseng processed product is carried out according to the following steps:
(1) preparation of control solutions: weighing a certain amount of ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rc and ginsenoside Rd, precisely weighing, and adding methanol to prepare a solution containing ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rc and ginsenoside Rd in each 1ml by the mass ratio of 0.06-0.08:0.6-0.75:1-1.2:0.1-0.12: 0.1-0.15;
(2) preparation of a test solution: weighing 1g of ginger-processed American ginseng, precisely weighing, precisely adding 50ml of water-saturated n-butanol, weighing, heating and refluxing in water bath for 1.5 hours, cooling, weighing again, supplementing the weight loss with water-saturated n-butanol, shaking up, and filtering; precisely measuring the subsequent filtrate, placing in an evaporating dish, evaporating to dryness, dissolving the residue with 50% methanol, transferring to a measuring flask, adding 50% methanol to scale, shaking, filtering, and collecting the subsequent filtrate;
(3) high performance liquid chromatography determination: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, measuring, and recording chromatogram; chromatographic conditions are as follows: using octadecylsilane chemically bonded silica as a filler, wherein a mobile phase comprises a mobile phase A and a mobile phase B, the mobile phase A is acetonitrile, the mobile phase B is 0.1% phosphoric acid solution, performing gradient elution, and detecting the wavelength of 203nm and the column temperature of 35 ℃.
Further, methanol is added to prepare the mixture containing ginsenoside Rg 10.063mg, ginsenoside Re 0.734mg, ginsenoside Rb 11.16mg, ginsenoside Rc 0.108mg and ginsenoside Rd 0.11mg per 1 ml;
further, methanol is added to prepare a solution containing ginsenoside Rg 10.08mg, ginsenoside Re 0.6mg, ginsenoside Rb 11mg, ginsenoside Rc 0.1mg and ginsenoside Rd 0.1mg per 1 ml;
further, the preparation of the reference substance solution in the step (1) also contains ginsenoside Rg2 and 6-gingerol, and methanol is added to prepare the reference substance solution containing ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rg2, ginsenoside Rc, ginsenoside Rd and 6-gingerol in a mass ratio of 0.063-0.08: 0.6-0.75: 1-1.2:0.1-0.4:0.1-0.12: 0.1-0.15: 0.004-0.006.
Further, methanol is added to prepare the mixture containing ginsenoside Rg 10.08mg, ginsenoside Re 0.6mg, ginsenoside Rb 11mg, ginsenoside Rg 20.2-0.35 mg, ginsenoside Rc 0.1mg, ginsenoside Rd 0.1mg and 6-gingerol 0.006mg per 1 ml;
further, methanol was added to make 1ml of the solution containing ginsenoside Rg 10.063mg, ginsenoside Re 0.734mg, ginsenoside Rb 11.160mg, ginsenoside Rg 20.334mg, ginsenoside Rc 0.108mg, ginsenoside Rd 0.11mg, 6-gingerol 0.006 mg;
further, (4) determination of characteristic peak relative retention time:
8 characteristic peaks exist in the characteristic spectrum of the test solution, the peak corresponding to the ginsenoside Rb1 is an S peak, the relative retention time of each characteristic peak and the S peak is calculated, and the relative retention time of each characteristic peak is respectively as follows: the relative retention time of the first characteristic peak is 0.661 +/-0.06, the relative retention time of the second characteristic peak is 0.64 +/-0.06, the relative retention time of the S peak is 1.00 +/-0.06, the relative retention time of the fourth characteristic peak is 1.02 +/-0.06, the relative retention time of the fifth characteristic peak is 1.03 +/-0.06, the relative retention time of the sixth characteristic peak is 1.08 +/-0.06, the relative retention time of the seventh characteristic peak is 1.11 +/-0.06 and the relative retention time of the eighth characteristic peak is 1.25 +/-0.06.
Further, the relative retention time of each characteristic peak is: the relative retention time of the first characteristic peak is 0.661 + -0.03, the relative retention time of the second characteristic peak is 0.64 + -0.03, the relative retention time of the S peak is 1.00 + -0.05, the relative retention time of the fourth characteristic peak is 1.02 + -0.05, the relative retention time of the fifth characteristic peak is 1.03 + -0.05, the relative retention time of the sixth characteristic peak is 1.08 + -0.05, the relative retention time of the seventh characteristic peak is 1.11 + -0.05, and the relative retention time of the eighth characteristic peak is 1.25 + -0.06.
Further, the S peak relative retention time was 1.00.
Further, (5) content measurement, obtaining a regression equation:
and (5) determining according to chromatographic conditions to obtain a linear regression equation.
Further, in the step (2) of preparing the test solution, 1g of ginger-processed American ginseng which is sieved by a third sieve is weighed and placed in a conical bottle with a plug.
Further, in the step (2), 25ml of the filtrate was precisely measured, placed in an evaporating dish, evaporated to dryness, and the residue was dissolved in a certain amount of 50% methanol and transferred to a 10ml measuring flask.
Further, the number of theoretical plates in the step (3) is not less than 600000 calculated according to the peak of ginsenoside Rb 1.
Further, the gradient elution conditions in step (3) are as follows:
Figure BDA0002218557690000031
further, the flow rate in step (3) was 1.0 ml/min.
Further, ginsenoside Rg1Ginsenoside Re and ginsenoside Rb1The content of the reference substance solution is more than or equal to 2.0 percent; the content of ginsenoside Rd and ginsenoside Rc in the reference solution is 0.2% or more.
The invention has the beneficial effects that:
(1) according to the characteristics of the processed ginger-processed American ginseng, the specificity identification and the multi-component and overall quality control are enhanced, the characteristic map of the variety can be established after content measurement, and further, the main content (Rg1, Re, Rb1, Rc, Rd and 6-gingerol) can be obtained by only one experiment for subsequent identification and the characteristic peaks (8 characteristic peaks) of the map can be obtained by comparison, so that the mass and comprehensive quality control is facilitated. The establishment of the characteristic spectrum has important practical significance for identifying the American ginseng and the ginger-processed American ginseng and improving and controlling the quality of the ginger-processed American ginseng.
(2) The invention provides the identification of the whole chemical components of the ginger-processed American ginseng, has strong specificity, increases the ginsenoside Rd, and has obvious difference from the content measurement of the ginsenoside Rc and the American ginseng.
(3) When only 0.1% phosphoric acid is added into the water phase, the number of peaks is large, the baseline is stable, and the separation degree is good (when 0.1% formic acid and 0.3% acetic acid are added into the water phase, the baseline of the chromatogram shifts seriously, and a peak appears at 5min, and the sample is not separated).
(4) The invention selects 1.0ml/min as the optimum flow rate, under the condition, the peak number of the atlas is more, and the target peak can reach the separation degree of 1.5 (under the flow rate condition of 0.8ml/min, the peak number is more, but the target peak separation degree is poorer, and the separation degree required by content determination can not be reached; under the flow rate condition of 1.2ml/min, the separation degree of each group of peaks is good, the peak is earlier, but the peak number is reduced, and the peak fusion exists).
(5) The invention selects 35 ℃ as the optimum column temperature, the peak number of the atlas is more under the condition, and the target peak can reach the separation degree of 1.5 (while the separation degree of the target peak is worse under the column temperature conditions of 0 ℃ and 40 ℃, and the separation degree required by content measurement can not be reached).
Drawings
FIG. 1a is a specific high performance liquid chromatogram of methanol;
FIG. 1b shows ginsenoside Rg1Ginsenoside Re and ginsenoside Rb1The specific high performance liquid chromatogram of the solution of the ginsenoside Rc, the ginsenoside Rd and the 6-gingerol mixed reference substance;
FIG. 1c is a high performance liquid chromatogram of a crude product of Panax quinquefolium;
FIG. 1d is a high performance liquid chromatogram of ginger;
FIG. 1e is a high performance liquid chromatogram of ginger-processed radix Panacis Quinquefolii;
FIG. 2 is a high performance liquid chromatogram of a control solution of the present invention at 87 min;
FIG. 3 is a 87min high performance liquid chromatogram of a sample solution of 20 batches of samples according to the invention;
FIG. 4 is a high performance liquid chromatogram of a control of characteristics of ginger-processed American ginseng of the present invention;
FIG. 5 is a linear relationship diagram of ginsenoside Rg1 solution;
FIG. 6 is a linear relationship of ginsenoside Re solution
FIG. 7 is a linear relationship diagram of ginsenoside Rb1 solution;
FIG. 8 is a linear relationship diagram of ginsenoside Rc solution;
FIG. 9 is a linear relationship diagram of ginsenoside Rd solution;
FIG. 10 is a linear relationship diagram of 6-gingerol solution;
wherein, 1: ginsenoside Rg1, 2: ginsenoside Re, 3: ginsenoside Rb1, 4: ginsenoside Rg2, 5: ginsenoside Rc, 6: unknown, 7: ginsenoside Rd, 8: 6-gingerol.
Detailed Description
The invention is further explained with reference to the drawings.
A quality control identification and content determination method for a ginger-processed American ginseng processed product is carried out according to the following steps:
preparation of control solutions: weighing ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rg2, ginsenoside Rc, ginsenoside Rd and 6-gingerol at a certain content, precisely weighing, and adding methanol to obtain a solution containing ginsenoside Rg 10.08mg, ginsenoside Re 0.6mg, ginsenoside Rb 11mg, ginsenoside Rg 20.2-0.35 mg, ginsenoside Rc 0.1mg, ginsenoside Rd 0.1mg and 6-gingerol 0.006mg per 1 ml;
(2) preparation of a test solution: weighing 1g of ginger-processed American ginseng passing through a third sieve, precisely weighing, placing in a conical flask with a plug, precisely adding 50ml of water-saturated n-butyl alcohol, weighing, placing in a water bath, heating, refluxing and extracting for 1.5 hours, cooling, weighing again, supplementing the weight loss by using water-saturated n-butyl alcohol, shaking uniformly, and filtering; precisely measuring 25ml of the subsequent filtrate, placing in an evaporating dish, evaporating to dryness, dissolving the residue with 50% methanol, transferring to a 10ml measuring flask, adding 50% methanol to the scale, shaking, filtering, and collecting the subsequent filtrate.
(3) High performance liquid chromatography determination: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, measuring, and recording chromatogram; chromatographic conditions are as follows: using octadecylsilane chemically bonded silica as a filler, wherein a mobile phase comprises a mobile phase A and a mobile phase B, the mobile phase A is acetonitrile, the mobile phase B is 0.1% phosphoric acid solution, performing gradient elution, and detecting the wavelength of 203nm and the column temperature of 35 ℃. The theoretical plate number is based on ginsenoside Rb1The peak should be no less than 600000. The flow rate in step (3) was 1.0 ml/min. The gradient elution conditions were:
TABLE 1 gradient elution schedule
Figure BDA0002218557690000051
Specificity control experiment
Preparation of a special reference solution: taking a proper amount of ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rc, ginsenoside Rd and 6-gingerol, precisely weighing, and adding methanol to prepare a reference solution stock solution containing ginsenoside Rg 10.08mg, ginsenoside Re 0.6mg, ginsenoside Rb 11mg, ginsenoside Rc 0.1mg, ginsenoside Rd 0.1mg and 6-gingerol 0.006mg per 1 ml.
According to the preparation method of the test solution, the ginger juice, the raw American ginseng solution and the ginger American ginseng solution are respectively prepared. Separating methanol, special reference solution, rhizoma Zingiberis recens solution, radix Panacis Quinquefolii solution, and rhizoma Zingiberis recens radix Panacis Quinquefolii solution, and obtaining special high performance liquid chromatogram shown in figures 1a-1 e.
FIG. 2 is a high performance liquid chromatogram of a control solution of the present invention at 87 min;
FIG. 3 is a 87min high performance liquid chromatogram of a sample solution of 20 batches of samples, wherein 1: ginsenoside Rg1, 2: ginsenoside Re, 3: ginsenoside Rb1, 4: ginsenoside Rg2, 5: ginsenoside Rc, 6: unknown, 7: ginsenoside Rd, 8: 6-gingerol.
The similarity of 20 batches of ginger-processed American ginseng samples is obtained, as shown in Table 2 below.
TABLE 220 evaluation of similarity of ginger-processed American ginseng
Figure BDA0002218557690000061
Table 2 shows that the samples of 20 batches of ginger-processed american ginseng have good similarity, which is greater than or equal to 0.95, and that the components of 20 batches of ginger-processed american ginseng have stable components and high quality consistency.
TABLE 320 retention time (min) of 8 characteristic peaks of ginger American ginseng
Figure BDA0002218557690000071
TABLE 420 relative retention time of 8 characteristic peaks of ginger-processed American Ginseng
Figure BDA0002218557690000081
Table 520 theoretical plate number table of 8 characteristic peaks of ginger American ginseng
Figure BDA0002218557690000091
Characteristic spectrum of ginger-processed American ginseng
The characteristic contrast high performance liquid chromatogram of radix Panacis Quinquefolii processed with ginger is shown in FIG. 4, and 8 characteristic peaks are determined, and reference substance of ginsenoside Rb1 of peak 3 is used to obtain characteristic contrast chromatogram data (Table 6).
The characteristic spectrum of the test sample should have 8 characteristic peaks, the peak corresponding to the reference peak of ginsenoside Rb1 is the S peak, the relative retention time of each characteristic peak and the S peak is calculated, and the specified values of the relative retention time of each characteristic peak are respectively: 0.661 (peak 1), 0.64 (peak 2)1.00(S peak), 1.02 (peak 4), 1.03 (peak 5), 1.08 (peak 6), 1.11 (peak 7), 1.25 (peak 8). The relative retention time of each characteristic peak in the chromatogram of the test sample has a variable range.
TABLE 6 characteristic map control map data
Figure BDA0002218557690000101
Standard curve of determination method for content of ginger-processed American ginseng
The chromatographic conditions and the specificity experiment in the content measurement are consistent with the method in the characteristic spectrum of the ginger-processed American ginseng.
Taking appropriate amount of ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rc, ginsenoside Rd and 6-gingerol, respectively, precisely weighing, and adding methanol to obtain a solution containing ginsenoside Rg 10.08mg, ginsenoside Re 0.6mg, ginsenoside Rb 11mg, ginsenoside Rc 0.1mg, ginsenoside Rd 0.1mg and 6-gingerol 0.006mg per 1 ml. Precisely sucking the stock solutions of the reference substances to prepare a mixed reference substance solution, and diluting to obtain a series of mixed reference substance solutions. The determination is carried out according to the chromatographic conditions of the invention.
Results and analysis
The mass of each control was plotted on the abscissa (X) and the peak area on the ordinate (Y), and the results of measurement were shown in FIGS. 5 to 10.
The solutions of the control samples all have a linear relationship at a certain concentration, and the regression equation is shown in Table 7.
TABLE 7 Linear regression equation Range for different controls
Figure BDA0002218557690000102
Precision experiment
Preparation of a reference solution: taking appropriate amount of ginsenoside Rg1 reference, ginsenoside Re reference, ginsenoside Rb1 reference, ginsenoside Rc reference, ginsenoside Rd reference and 6-gingerol reference, and continuously sampling for 6 times according to the chromatographic condition of the invention to obtain Table 8.
Results and analysis
TABLE 8 results of precision test
Figure BDA0002218557690000111
Ginsenoside Rg1Ginsenoside Re and ginsenoside Rb1The peak areas RSD of the ginsenoside Rc, the ginsenoside Rd and the 6-gingerol are all less than 3.0 percent, which indicates that the precision of the instrument is good.
Stability test
Ginger-processed American ginseng solution was prepared according to the method of the present invention, and the chromatographic conditions of the present invention were measured at 0, 4, 8, 12, 16, 20, and 24h after the preparation, to obtain Table 9.
Results and analysis
TABLE 9 stability test results
Figure BDA0002218557690000112
GinsenosideRg1Ginsenoside Re and ginsenoside Rb1The peak areas RSD of the ginsenoside Rc, the ginsenoside Rd and the 6-gingerol are all less than 3.0 percent, which indicates that the test solution has good stability within 24 hours.
Repeatability test
6 parts of the same batch of ginger-processed American ginseng solution is prepared, and 6 parts of samples are measured according to the chromatographic conditions of the invention, thus obtaining the table 10.
Results and analysis
TABLE 10 results of the repeatability tests
Figure BDA0002218557690000121
Ginsenoside Rg1Ginsenoside Re and ginsenoside Rb1The contents RSD of the ginsenoside Rc, the ginsenoside Rd and the 6-gingerol are all less than 3.0 percent, which shows that the method has good repeatability.
Sample application recovery rate test
Experimental methods
Collecting 0.5g rhizoma Zingiberis recens radix Panacis Quinquefolii powder, and adding ginsenoside Rg into the powder1Ginsenoside Re and ginsenoside Rb1And appropriate amounts of ginsenoside Rc, ginsenoside Rd and 6-gingerol are added, so that the ratio of the concentration of the added reference substance to the concentration of the component to be detected in the sample is respectively 1: 1, 6 parts of sample solution of the same lot are prepared according to the method of the invention, and six samples are measured under chromatographic conditions, thus obtaining tables 11-16.
Results and analysis
TABLE 11 ginsenoside Rg1Results of recovery test
Figure BDA0002218557690000122
TABLE 12 ginsenoside Re recovery test results
Figure BDA0002218557690000131
TABLE 13 ginsenoside Rb1Results of recovery test
Figure BDA0002218557690000132
TABLE 14 sample recovery test results for ginsenoside Rc
Figure BDA0002218557690000133
TABLE 15 ginsenoside Rd recovery test results
Figure BDA0002218557690000134
TABLE 166-gingerol recovery test results
Figure BDA0002218557690000141
Ginsenoside Rg1Ginsenoside Re and ginsenoside Rb1The sample adding recovery rates RSD of the ginsenoside Rc, the ginsenoside Rd and the 6-gingerol are respectively 2.152%, 2.995%, 2.955%, 2.989%, 1.098% and 2.934%, and are all less than 3%, which indicates that the recovery rate of the method is good.
The invention obtains the content result of 20 batches of ginger-processed American ginseng samples
TABLE 17 determination of the content of each component (%)
Figure BDA0002218557690000142
The product contains ginsenoside Rg1(C42H72O14) Ginsenoside Re (C)48H82O18) Ginsenoside Rb1(C54H92O23) The total content of ginsenoside Rd (C) should not be less than 2.0%48H82O18) And ginsenoside Rc (C)53H90O22) The total content of (A) should not be less than 0.2%. Because the content of the 6-gingerol is low, the content is not listed under the content measurement item.
Although the present invention has been described with reference to a preferred embodiment, it should be understood that various changes, substitutions and alterations can be made herein without departing from the spirit and scope of the invention as defined by the appended claims.

Claims (6)

1. A quality identification and determination method for a ginger-processed American ginseng processed product is characterized by comprising the following steps:
(1) preparation of control solutions: weighing ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rg2, ginsenoside Rc, ginsenoside Rd and 6-gingerol at a certain content, precisely weighing, and adding methanol to obtain a solution containing ginsenoside Rg 10.08mg, ginsenoside Re 0.6mg, ginsenoside Rb 11mg, ginsenoside Rg 20.2-0.35 mg, ginsenoside Rc 0.1mg, ginsenoside Rd 0.1mg and 6-gingerol 0.006mg per 1 ml;
(2) preparation of a test solution: weighing 1g of ginger-processed American ginseng, precisely weighing, precisely adding 50ml of water-saturated n-butanol, weighing, heating and refluxing in water bath for 1.5 hours, cooling, weighing again, supplementing the weight loss with water-saturated n-butanol, shaking up, and filtering; precisely measuring the subsequent filtrate, placing in an evaporating dish, evaporating to dryness, dissolving the residue with 50% methanol, transferring to a measuring flask, adding 50% methanol to scale, shaking, filtering, and collecting the subsequent filtrate;
(3) high performance liquid chromatography determination: precisely sucking 10 μ l of each of the reference solution and the sample solution, injecting into a liquid chromatograph, measuring, and recording chromatogram; chromatographic conditions are as follows: using octadecylsilane chemically bonded silica as a filler, wherein a mobile phase consists of a mobile phase A and a mobile phase B, the mobile phase A is acetonitrile, the mobile phase B is 0.1% phosphoric acid solution, performing gradient elution, and detecting the wavelength of 203nm and the column temperature of 35 ℃;
(4) determination of characteristic peak relative retention time:
8 characteristic peaks exist in the characteristic spectrum of the test solution, the peak corresponding to the ginsenoside Rb1 is an S peak, the relative retention time of each characteristic peak and the S peak is calculated, and the relative retention time of each characteristic peak is respectively as follows: the relative retention time of the first characteristic peak is 0.661 +/-0.06, the relative retention time of the second characteristic peak is 0.64 +/-0.06, the relative retention time of the S peak is 1.00 +/-0.06, the relative retention time of the fourth characteristic peak is 1.02 +/-0.06, the relative retention time of the fifth characteristic peak is 1.03 +/-0.06, the relative retention time of the sixth characteristic peak is 1.08 +/-0.06, the relative retention time of the seventh characteristic peak is 1.11 +/-0.06 and the relative retention time of the eighth characteristic peak is 1.25 +/-0.06;
the number of theoretical plates in the step (3) is not less than 600000 calculated according to the peak of ginsenoside Rb 1;
the gradient elution conditions in the step (3) are as follows:
Figure FDA0003470876210000021
2. the method for identifying and measuring the quality of the processed ginger-processed American ginseng product according to claim 1, wherein the method comprises the following steps: the relative retention time of each characteristic peak is respectively as follows: the relative retention time of the first characteristic peak is 0.661 + -0.03, the relative retention time of the second characteristic peak is 0.64 + -0.03, the relative retention time of the S peak is 1.00 + -0.05, the relative retention time of the fourth characteristic peak is 1.02 + -0.05, the relative retention time of the fifth characteristic peak is 1.03 + -0.05, the relative retention time of the sixth characteristic peak is 1.08 + -0.05, the relative retention time of the seventh characteristic peak is 1.11 + -0.05, and the relative retention time of the eighth characteristic peak is 1.25 + -0.06.
3. The method for identifying and measuring the quality of the processed ginger-processed American ginseng product according to claim 1, wherein the method comprises the following steps:
(5) and (4) content measurement, obtaining a regression equation:
and (5) determining according to chromatographic conditions to obtain a linear regression equation.
4. The method for identifying and measuring the quality of the processed ginger-processed American ginseng product according to claim 1, wherein the method comprises the following steps: weighing 1g of ginger-processed American ginseng which is sieved by a third sieve in the preparation of the test solution in the step (2) and placing the ginger-processed American ginseng in a conical bottle with a plug.
5. The method for identifying and measuring the quality of the processed ginger-processed American ginseng product according to claim 1, wherein the method comprises the following steps: and (3) precisely measuring 25ml of the subsequent filtrate in the step (2), placing the subsequent filtrate in an evaporating dish, evaporating to dryness, adding a certain amount of 50% methanol into the residue to dissolve the residue, and transferring the residue into a 10ml measuring flask.
6. The method for identifying and measuring the quality of the processed ginger American ginseng product according to claim 1 or 3, wherein the method comprises the following steps: the flow rate in step (3) was 1.0 ml/min.
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