CN113640413B - Method for detecting Chinese and western ginseng components in ginseng spleen-invigorating pills - Google Patents
Method for detecting Chinese and western ginseng components in ginseng spleen-invigorating pills Download PDFInfo
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Abstract
The invention discloses a method for detecting Chinese and western ginseng components in a ginseng spleen-invigorating pill, which comprises a high performance liquid chromatography-evaporative light scattering detector inspection method and a high performance liquid chromatography-tandem mass spectrometry inspection method. The method for detecting the components of the American ginseng and the Chinese western medicine in the ginseng spleen-invigorating pill can effectively improve the accuracy and the stability of sample detection through a reasonable detection method, parameter design and complete sample pretreatment measures, is convenient to popularize and use, can be used for detecting by two detection methods at the same time, and has strong applicability.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine detection, and particularly relates to a method for detecting Chinese and western ginseng components in a ginseng spleen-invigorating pill.
Background
The Ginseng radix GUIPI pill is prepared from modified GUIPI pill Fang Erlai from Song dynasty' Ji Sheng Fang, and the prescription is composed of ten kinds of medicines such as Ginseng radix, radix astragali, radix Angelicae sinensis, arillus longan, and semen Ziziphi Spinosae. Has effects in invigorating qi and tonifyingBlood, spleen and heart. Ginseng is sweet and slightly bitter in taste, warm and mild in nature. It enters spleen, lung and heart meridians. Invigorating qi, relieving depletion, promoting salivation, tranquilizing, and improving intelligence; the main chemical components comprise saponins, flavonoids, volatile oils and the like. According to Chinese pharmacopoeia, ginseng and American ginseng contain ginsenoside Rg1, re and Rb1, ginseng contains ginsenoside Rf as characteristic component, and American ginseng contains pseudoginsenoside F as characteristic component 11 . In order to strictly control the quality of the product, it is necessary to control the quality of ginseng in the prescription.
The existing standard lacks a special detection method for the ginseng adulteration component (American ginseng) in the ginseng spleen-invigorating pill, and the ginseng adulteration detection method of other preparations is not reasonable enough, has narrow applicability, is not perfect for the pretreatment of samples, influences the accuracy and stability of final detection, and is not convenient for popularization and use.
In summary, how to design a method for detecting the components of the American ginseng, the Chinese ginseng and the western ginseng in the ginseng spleen-invigorating pill can effectively improve the accuracy and the stability of sample detection, is convenient for popularization and use, and is a problem which needs to be solved urgently at present.
Disclosure of Invention
The invention aims to solve the technical problems, and provides a method for detecting the ingredients of American ginseng and western ginseng in ginseng spleen-invigorating pills, which has reasonable detection method and parameter design, through perfect sample pretreatment measures, on one hand, a semipermeable membrane is designed to remove honey in a ginseng spleen-invigorating pill sample, on the other hand, the impurity removal effect is improved through the modification of a filter membrane in a sample filter, the accuracy and the stability of sample detection can be effectively improved, the popularization and the use are convenient, and the method can be simultaneously used for detecting by a high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) detection method and a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) detection method, and has strong applicability.
The invention realizes the aim through the following technical scheme, and the method for detecting the Chinese and western ginseng components in the ginseng spleen-invigorating pill comprises the following steps:
(1) Preparation of a test solution:
a. removing honey in the ginseng spleen-invigorating pills: taking 2 pills of ginseng spleen-invigorating pills, cutting into pieces, adding 50ml water, stirring for 10-15min at 40-45 ℃, then filtering, respectively collecting solid residues and filtrate, dialyzing the filtrate by using a semipermeable membrane to remove monosaccharide molecules, and mixing the obtained product with the solid residues to obtain a material to be detected;
b. taking the material to be tested, adding 100ml of water saturated n-butyl alcohol, heating and refluxing for 1 hour, filtering, washing the filtrate with ammonia test solution for 2 times, 50ml each time, discarding the ammonia washing solution, taking the n-butyl alcohol solution, washing with 50ml of water saturated with n-butyl alcohol, taking the n-butyl alcohol layer to dry, dissolving the residue with methanol 2 ml, filtering with a sample filter, and taking the subsequent filtrate as a test sample solution;
(2) Preparation of control solutions:
collecting pseudoginsenoside F 11 Accurately weighing reference substance, and adding methanol to obtain reference substance solution;
(3) Preparation of negative control solution:
taking a ginseng-lacking medicinal material, preparing a negative control sample according to a prescription process, weighing 18 g, and preparing a ginseng-lacking negative control solution by the same method as the preparation method of the test sample solution;
(4) The measuring method comprises the following steps:
detecting by high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) or high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), setting detection conditions, respectively absorbing 10-20 μ L of test solution, control solution and negative control solution, and performing sample injection;
(5) And (5) judging a result:
in the chromatogram of the test sample, no chromatographic peak with the same retention time as that of the chromatographic peak of the reference sample should appear.
Further, the step (4) is detected by a high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) detection method, and the chromatographic conditions are as follows: a chromatographic column: capcell pak C18 (4.6 mm X250 mm,5 μm), mobile phase: acetonitrile-water (volume ratio 30; evaporative light scattering detector: gas flow rate: 1.6 L/min, flow rate: 1ml/min, and the column temperature is 30 ℃;
in this case, the preparation method of the reference solution in the step (2) is as follows: precision scaleCollecting pseudoginsenoside F 11 And (3) placing a reference substance 10.05 mg in a 50ml measuring flask, adding methanol to dissolve and dilute to a scale mark, and shaking uniformly to obtain a reference substance solution.
Further, the step (4) adopts a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) inspection method for detection, and the chromatographic conditions are as follows:
chromatographic column Waters ACQUITY UPLC BEH-C 18 (2.1 mm. Times.100 mm,1.7 μm); acetonitrile is taken as a mobile phase A, and water is taken as a mobile phase B; the flow rate is 0.4 ml/min; the column temperature is 40 ℃; 3 mu L of sample volume;
gradient elution: 0-12 min, 8-80% A; for 12-14 min, 80-90% of A; 14-14.2 min, 90-8% A; 14.2-20 min,8% A; the volume ratio of acetonitrile to water is 30;
the mass spectrum conditions are as follows: taking a flight time mass spectrum as a detector, adopting an electrospray ionization ion source and a negative ion mode for detection, taking Leucine-enkephalin as a calibration solution, and scanning the range: m/z is 50-1200, the sampling interval is 0.5s, the capillary voltage is 2.5kV, the taper hole voltage is 40V, the ion source temperature is 100 ℃, the desolvation temperature is 450 ℃, and the desolvation gas flow rate is 800 L.h -1 And the flow rate of the conical hole is 40 L.h -1 The collision gas is argon; the collision low energy is 6V, and the collision high energy is 20-40V;
in this case, the preparation method of the reference solution in the step (2) is as follows: collecting pseudoginsenoside F 11 And (3) precisely weighing a reference substance, adding methanol to prepare a solution containing 50 microgram per 1ml, and shaking up to obtain the reference substance solution.
Further, the preparation method of the semipermeable membrane in the step (1) comprises the following steps:
A. mixing the alkaline basalt nano powder with 0.1-0.3 times of silicone oil, placing the mixture in a dispersion machine of 1000-2000r/min for dispersing for 1-2h to obtain nano powder, and mixing the nano powder with 40-60 times of water to prepare dispersion liquid;
B. and (2) taking a certain amount of filter paper, immersing the filter paper in 75% cold sulfuric acid by using a glass rod for 70-80s, taking out the filter paper, spraying a saturated carbonic acid solution on the surface of the filter paper, wherein the spraying amount is 6-10%, after the spraying is finished, putting the filter paper into the dispersion liquid obtained in the step (A) for rinsing for 1-3 times, then putting the filter paper into dilute ammonia water for soaking for 3-5min, taking out and airing to obtain the semipermeable membrane.
Further, the filtering membrane of the sample filter in the step (1) is a modified regenerated cellulose filtering membrane, and the pore diameter of the modified regenerated cellulose filtering membrane is 0.2-0.5 μm.
Further, the preparation method of the modified regenerated cellulose filter membrane comprises the following steps:
s1, preparing a controlled release pore-forming agent: granulating the pore-forming agent for later use, dissolving poly N2 isopropyl acrylamide in deionized water at 24-26 ℃ to prepare material liquid, spraying the obtained material liquid on the surface of the granulated pore-forming agent at 31-33 ℃ and 1-1.5MPa, then heating to 40-50 ℃ and preserving heat for 20-30min to obtain the controlled-release pore-forming agent;
s2, preparing a membrane preparation liquid: dissolving cellulose in a solvent, then adding polylactic acid, a controlled-release pore-forming agent and an additive, uniformly mixing, defoaming and filtering to obtain a membrane-making solution;
s3, film making: and (2) casting the membrane-making liquid prepared in the step (S2) on a glass plate to form a flat membrane at the temperature of 80-84 ℃, standing the flat membrane for 3-5S at the temperature of 40-50 ℃ in an aeration environment, stopping aeration, cooling the flat membrane to below 30 ℃, standing for 30-50min, standing for 5-10S in the aeration environment, then putting the flat membrane into a coagulating bath, solidifying for 10-15min to form a membrane, washing away residual solvent in the membrane by deionized water, and airing at room temperature to obtain the modified regenerated cellulose filtering membrane.
Further, in the step S1, the mass ratio of the material liquid to the pore-forming agent is (0.08-0.12): 1, the mass concentration of poly N2 isopropyl acrylamide in the material liquid is 4-8%; in the step S2, the mass ratio of the cellulose to the polylactic acid to the controlled-release pore-forming agent to the additive is 1: (0.3-0.6): (0.15-0.3): (0.02-0.05).
Further, in step S1, the pore-forming agent includes a pore-forming agent a and a pore-forming agent B, and the mass ratio of the pore-forming agent a to the pore-forming agent B is 1: (0.3-0.6), the pore-forming agent A and the pore-forming agent B are separately granulated, the pore-forming agent A is polyethylene glycol, the pore-forming agent B is sodium chloride and sodium alginate, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1: (1.5-3).
Further, the air conditioner is provided with a fan,the solvent in the step S2 is prepared from (2-4): 1, dimethyl sulfoxide/tetraethylammonium chloride, wherein the additive is fatty glyceride or polysorbate; the aeration environment in step S3 is: nitrogen or argon with a ventilation of 0.05-0.1m 3 /h。
The invention also discloses application of the detection method in controlling the quality of the ginseng in the ginseng spleen-invigorating pills.
The invention has the beneficial effects that:
(1) The invention can effectively improve the accuracy and stability of sample detection through reasonable detection method and parameter design and perfect sample pretreatment measures, is convenient for popularization and use, can be simultaneously used for detection by a high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) detection method and a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) detection method, and has strong applicability;
(2) Because the target sample ginseng spleen-invigorating pill contains a large amount of honey, the honey in the ginseng spleen-invigorating pill is removed by adopting a semipermeable membrane during sample pretreatment, so that the adverse effect of the honey in subsequent detection can be reduced;
(3) The surface of the semipermeable membrane prepared by the invention contains the nano powder prepared by mixing the alkaline basalt nano powder and the silicone oil, so that the smoothness of the surface of the semipermeable membrane can be improved, and the adsorption and loss of a sample are reduced in the process of removing monosaccharide molecules through dialysis, so that the accuracy is improved;
(4) When the semipermeable membrane is prepared, the alkaline basalt nano powder is selectively introduced into the surface of the semipermeable membrane, the alkaline content in the alkaline basalt is high, more concentrated sulfuric acid is remained on the surface of the filter paper after reaction in the concentrated sulfuric acid, at the moment, the alkaline basalt nano powder is introduced into the surface of the filter paper, the tight combination of the nano powder and the surface of the filter paper can be enhanced, in addition, the alkaline basalt nano powder has good fluidity and lubricity, and the smoothness of the surface of the semipermeable membrane can be enhanced;
(5) When the semipermeable membrane is prepared, the silicone oil and the alkaline basalt nano powder are dispersed at a high speed to prepare the nano powder, on one hand, the silicone oil can form an ultra-smooth surface after filling pores of the alkaline basalt nano powder, and on the other hand, the silicone oil is a non-polar substance and can further reduce sample adsorption and loss after being introduced to the surface of the semipermeable membrane;
(6) In the step B of preparing the semipermeable membrane, after the surface of the filter paper is hydrolyzed, a saturated carbonic acid solution is sprayed on the surface of the filter paper, so that the process that sodium carbonate is decomposed to release carbon dioxide when rinsing is carried out in subsequent dispersion liquid, the material exchange on the surface of the filter paper is promoted, and the combination of the nano powder in the dispersion liquid and the surface of the filter paper is promoted;
(7) Because the impurity content of the sample has great influence on the detection process, the filtering membrane of the sample filter adopts a modified regenerated cellulose filtering membrane, the main preparation materials are cellulose and polylactic acid, and the sample filter is an environment-friendly degradable material and is suitable for disposable use in a laboratory;
(8) According to the modified regenerated cellulose filtering membrane prepared by the invention, the preparation and addition of the controlled-release pore-forming agent can control the pore-forming time, the pore-forming agent is more uniformly distributed, the porosity of the membrane can be effectively improved, the size of membrane pores is uniform, the filtering efficiency is high, and impurities can be effectively removed;
(9) When the modified regenerated cellulose filtering membrane is prepared, the adopted pore-forming agent consists of a pore-forming agent A and a pore-forming agent B, the pore-forming agent A is polyethylene glycol and can enhance the membrane flux, the pore-forming agent B is sodium chloride and sodium alginate, when the outer layer coating material poly N2 isopropyl acrylamide gel is melted below 30 ℃, the water in the gel, the sodium chloride and the sodium alginate are released, so that the sodium alginate plays the role of the pore-forming agent in a sodium chloride aqueous solution and forms a large number of pores in the membrane, and the pore-forming agent A and the pore-forming agent B are matched together, so that the membrane performance of the modified regenerated cellulose filtering membrane can be obviously improved.
Drawings
FIG. 1 shows pseudoginsenoside F 11 A control chromatogram;
FIG. 2 is a negative control sample chromatogram;
FIG. 3 is a chromatogram of a sample (A Enterprise sample, lot number 17013851);
FIG. 4 is a chromatogram of a sample (sample from Enterprise B, lot number 20170205);
FIG. 5 shows pseudoginsenoside F 11 A full-scan base peak map;
FIG. 6 shows pseudoginsenoside F 11 A primary mass spectrogram;
FIG. 7 shows pseudoginsenoside F 11 A secondary mass spectrum;
FIG. 8 is a full scan base peak plot of a negative control sample;
FIG. 9 is a full scan base peak chart of the test sample (sample of Enterprise B, lot number 20170205);
FIG. 10 is a primary mass spectrum of a sample (sample of Enterprise B, lot number 20170205);
FIG. 11 is a secondary mass spectrum of the sample (sample from Enterprise B, lot number 20170205).
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention.
Instrument and reagent kit
1. Instrument for measuring the position of a moving object
Agilent 1260 high performance liquid chromatograph; agilent Technologies ELSD detector; acquity UPLC/Xevo G2 QT of liquid chromatograph-analyzer, massLynx V4.1 Mass Spectroscopy workstation (Waters Corp.); sartorius BT 25S electronic balance.
2. Reagent
Ginseng spleen-invigorating pills: A. and 10 batches of samples (big honeyed pills) in the B enterprise.
Negative control samples: taking the raw and auxiliary materials of the ginseng lacking medicinal material, and preparing a negative sample according to the preparation process of the product.
Pseudo-ginseng saponin F 11 : the source is as follows: china food and drug testing research institute batch number: 110841-201607.
Acetonitrile is chromatographically pure, and the experimental water is deionized water.
Example 1
The embodiment provides a method for detecting the components of American ginseng in Chinese and western ginseng pills, which comprises the following steps:
(1) Preparation of a test solution:
a. removing honey in the ginseng spleen-invigorating pills: taking 2 pills of ginseng spleen-invigorating pills, cutting into pieces, adding 50ml water, stirring for 10min at 40 ℃, then filtering, respectively collecting solid residues and filtrate, dialyzing the filtrate by using a semipermeable membrane to remove monosaccharide molecules, and mixing the obtained product with the solid residues to obtain a material to be detected;
b. taking the material to be tested, adding 100ml of water saturated n-butyl alcohol, heating and refluxing for 1 hour, filtering, washing the filtrate with ammonia test solution for 2 times, 50ml each time, discarding the ammonia washing solution, taking the n-butyl alcohol solution, washing with 50ml of water saturated with n-butyl alcohol, taking the n-butyl alcohol layer to dry, dissolving the residue with methanol 2 ml, filtering with a sample filter, and taking the subsequent filtrate as a test sample solution;
(2) Preparation of control solutions:
accurately weighing pseudoginsenoside F 11 Placing a reference substance 10.05 mg in a 50ml measuring flask, adding methanol to dissolve and dilute to scale, and shaking uniformly to obtain a reference substance solution;
(3) Preparation of negative control solution:
taking a ginseng-lacking medicinal material, preparing a negative control sample according to a prescription process, weighing 18 g, and preparing a ginseng-lacking negative control solution by the same method as the preparation method of the test sample solution;
(4) The determination method comprises the following steps:
detecting by high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) detection method, setting detection conditions, respectively sucking 10 μ L of sample solution, control solution, and negative control solution, and detecting by sample injection;
(5) And (5) judging a result:
in the chromatogram of the test sample, a chromatographic peak with the same retention time as that of the chromatographic peak of the reference substance cannot appear.
In the step (4), the chromatographic conditions are as follows: a chromatographic column: capcell pak C18 (4.6 mm X250 mm,5 μm), mobile phase: acetonitrile-water (volume ratio 30; evaporative light scattering detector: gas flow rate: 1.6 L/min, flow rate: 1ml/min, and the column temperature is 30 ℃.
Example 2
The embodiment provides a method for detecting Chinese and western ginseng components in a ginseng spleen-invigorating pill, which comprises the following steps:
(1) Preparation of a test solution:
a. removing honey in the ginseng spleen-invigorating pills: taking 2 pills of ginseng spleen-invigorating pills, cutting into pieces, adding 50ml water, stirring for 15min at 45 ℃, then filtering, respectively collecting solid residues and filtrate, dialyzing the filtrate by using a semipermeable membrane to remove monosaccharide molecules, and mixing the obtained product with the solid residues to obtain a material to be detected;
b. taking the material to be tested, adding 100ml of water saturated n-butyl alcohol, heating and refluxing for 1 hour, filtering, washing the filtrate with ammonia test solution for 2 times, 50ml each time, discarding the ammonia washing solution, taking the n-butyl alcohol solution, washing with 50ml of water saturated with n-butyl alcohol, taking the n-butyl alcohol layer to dry, dissolving the residue with methanol 2 ml, filtering with a sample filter, and taking the subsequent filtrate as a test sample solution;
(2) Preparation of control solutions:
collecting pseudoginsenoside F 11 Precisely weighing a reference substance, adding methanol to prepare a solution containing 50 microgram per 1ml, and shaking up to obtain a reference substance solution;
(3) Preparation of negative control solution:
taking a ginseng-lacking medicinal material, preparing a negative control sample according to a prescription process, weighing 18 g, and preparing a ginseng-lacking negative control solution by the same method as the preparation method of the test sample solution;
(4) The determination method comprises the following steps:
detecting by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), setting detection conditions, respectively sucking 20 μ L of test solution, control solution and negative control solution, and performing sample injection detection;
(5) And (5) judging a result:
in the chromatogram of the test sample, a chromatographic peak with the same retention time as that of the chromatographic peak of the reference substance cannot appear.
In the step (4), the chromatographic conditions are as follows:
chromatographic column Waters ACQUITY UPLC BEH-C 18 (2.1 mm. Times.100 mm,1.7 μm); acetonitrile is taken as a mobile phase A, and water is taken as a mobile phase B; the flow rate is 0.4 ml/min; the column temperature is 40 ℃; 3 mu L of sample volume;
gradient elution: 0-12 min,8% -80% A; for 12-14 min, 80-90% of A; 14-14.2 min, 90-8% A; 14.2-20 min,8% A; the volume ratio of acetonitrile to water is 30;
the mass spectrum conditions are as follows: taking a flight time mass spectrum as a detector, adopting an electrospray ionization ion source and a negative ion mode for detection, taking Leucine-enkephalin as a calibration solution, and scanning the range: m/z is 50-1200, the sampling interval is 0.5s, the capillary voltage is 2.5kV, the taper hole voltage is 40V, the ion source temperature is 100 ℃, the desolvation temperature is 450 ℃, and the desolvation gas flow rate is 800 L.h -1 And the flow rate of the conical hole is 40 L.h -1 The collision gas is argon; the collision low energy is 6V, and the collision high energy is 20-40V.
Example 3
On the basis of the embodiment 1, the embodiment also provides a method for detecting the ingredients of the western ginseng in the ginseng spleen-invigorating pill, and the preparation method of the semipermeable membrane in the step (1) comprises the following steps:
A. mixing alkaline basalt nano powder with 0.1 time of silicone oil, then placing the mixture into a dispersion machine with the speed of 1000r/min for dispersion for 1 hour to obtain nano powder, and mixing the nano powder with 40 times of water to prepare dispersion liquid;
B. and (3) taking a certain amount of filter paper, immersing the filter paper in 75% cold sulfuric acid by using a glass rod, taking out the filter paper after 70s of immersion, spraying a saturated carbonic acid solution on the surface of the filter paper, wherein the spraying amount is 6%, putting the filter paper into the dispersion liquid obtained in the step A to rinse for 1 time after the spraying is finished, putting the filter paper into dilute ammonia water to soak for 3min, taking out and airing to obtain the semipermeable membrane.
The rest is the same as in example 1.
Example 4
On the basis of the embodiment 2, the embodiment also provides a method for detecting the ingredients of the western ginseng in the ginseng spleen-invigorating pill, and the preparation method of the semipermeable membrane in the step (1) comprises the following steps:
A. mixing alkaline basalt nano powder with 0.3 times of silicone oil, placing the mixture in a 2000r/min dispersion machine for dispersing for 2 hours to obtain nano powder, and mixing the nano powder with 60 times of water to prepare dispersion liquid;
B. and (2) taking a certain amount of filter paper, immersing the filter paper in 75% cold sulfuric acid by using a glass rod, taking out the filter paper after soaking for 80s, spraying a saturated carbonic acid solution on the surface of the filter paper, wherein the spraying amount is 10%, putting the filter paper into the dispersion liquid obtained in the step A after spraying, rinsing for 3 times, putting the filter paper into dilute ammonia water, soaking for 5min, taking out and drying to obtain the semipermeable membrane.
The rest is the same as in example 2.
Example 5
On the basis of the embodiment 1, the embodiment also provides a method for detecting the ingredients of the western ginseng and the Chinese ginseng in the ginseng-spleen-invigorating pill, wherein the filtering membrane of the sample filter in the step (1) is a modified regenerated cellulose filtering membrane, and the pore diameter of the modified regenerated cellulose filtering membrane is 0.2 μm.
The preparation method of the modified regenerated cellulose filter membrane comprises the following steps:
s1, preparing a controlled release pore-forming agent: granulating the pore-forming agent for later use, dissolving poly N2 isopropyl acrylamide in deionized water at 24 ℃ to prepare a material liquid, spraying the obtained material liquid on the surface of the granulated pore-forming agent at 31 ℃ and 1MPa, heating to 40 ℃ and preserving heat for 20min to obtain the controlled-release pore-forming agent;
s2, preparing a membrane preparation liquid: dissolving cellulose in a solvent, then adding polylactic acid, a controlled-release pore-forming agent and an additive, uniformly mixing, defoaming and filtering to obtain a membrane-making solution;
s3, film making: and (3) casting the film-forming liquid prepared in the step (S2) on a glass plate to form a flat membrane at the temperature of 80 ℃, standing the flat membrane for 3S at the temperature of 40 ℃ in an aeration environment, stopping aeration, cooling the flat membrane to the temperature below 30 ℃, standing for 30min, standing for 5S in the aeration environment, putting the flat membrane into a coagulating bath, curing for 10min to form a membrane, washing away residual solvent in the membrane by using deionized water, and airing at room temperature to obtain the modified regenerated cellulose filtering membrane.
In the step S1, the mass ratio of the material liquid to the pore-forming agent is 0.08:1, the mass concentration of poly N2 isopropyl acrylamide in the material liquid is 4%; in the step S2, the mass ratio of the cellulose to the polylactic acid to the controlled-release pore-forming agent to the additive is 1:0.3:0.15:0.02.
in the step S1, the pore-forming agent comprises a pore-forming agent A and a pore-forming agent B, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1:0.3, granulating the pore-forming agent A and the pore-forming agent B separately, wherein the pore-forming agent A is polyethylene glycol, the pore-forming agent B is sodium chloride and sodium alginate, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1:1.5.
the solvent in the step S2 is prepared from the following components in proportion of 2:1, dimethyl sulfoxide/tetraethyl ammonium chloride, and an additive is fatty glyceride; the aeration environment in step S3 is: nitrogen gas, ventilation volume 0.05 m 3 /h。
The rest is the same as in example 1.
Example 6
On the basis of the embodiment 2, the embodiment also provides a method for detecting the ingredients of the western ginseng and the Chinese ginseng in the ginseng-spleen-invigorating pill, wherein the filtering membrane of the sample filter in the step (1) is a modified regenerated cellulose filtering membrane, and the pore diameter of the modified regenerated cellulose filtering membrane is 0.5 μm.
The preparation method of the modified regenerated cellulose filter membrane comprises the following steps:
s1, preparing a controlled release pore-forming agent: granulating the pore-forming agent for later use, dissolving poly N2 isopropyl acrylamide in deionized water at 26 ℃ to prepare a material liquid, spraying the obtained material liquid on the surface of the granulated pore-forming agent at 33 ℃ and 1.5MPa, heating to 50 ℃ and preserving heat for 30min to obtain the controlled-release pore-forming agent;
s2, preparing a membrane preparation liquid: dissolving cellulose in a solvent, then adding polylactic acid, a controlled-release pore-forming agent and an additive, uniformly mixing, defoaming and filtering to obtain a membrane-making solution;
s3, film making: and (3) casting the membrane-forming liquid prepared in the step (S2) on a glass plate to form a flat membrane at the temperature of 84 ℃, standing the flat membrane for 5S at the temperature of 50 ℃ in an aeration environment, stopping aeration, cooling the flat membrane to the temperature below 30 ℃, standing for 50min, standing for 10S in the aeration environment, putting the flat membrane into a coagulating bath, curing for 15min to form a membrane, washing away residual solvent in the membrane with deionized water, and airing at room temperature to obtain the modified regenerated cellulose filtering membrane.
In the step S1, the mass ratio of the material liquid to the pore-forming agent is 0.12:1, the mass concentration of poly N2 isopropyl acrylamide in the material liquid is 8%; in the step S2, the mass ratio of the cellulose to the polylactic acid to the controlled-release pore-forming agent to the additive is 1:0.6:0.3: 0.05.
In the step S1, the pore-forming agent comprises a pore-forming agent A and a pore-forming agent B, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1:0.6, granulating the pore-forming agent A and the pore-forming agent B separately, wherein the pore-forming agent A is polyethylene glycol, the pore-forming agent B is sodium chloride and sodium alginate, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1:3.
the solvent in the step S2 is prepared from the following components in proportion of 4:1 dimethyl sulfoxide/tetraethyl ammonium chloride, and the additive is polysorbate; the ventilation environment in step S3 is: argon gas with a ventilation of 0.1m 3 /h。
The rest is the same as in example 2.
Example 7
The embodiment provides a method for detecting Chinese and western ginseng components in a ginseng spleen-invigorating pill, which comprises the following steps:
(1) Preparation of a test solution:
a. removing honey in the ginseng spleen-invigorating pills: taking 2 pills of ginseng spleen-invigorating pills, cutting into pieces, adding 50ml water, stirring for 12min at 42 ℃, then filtering, respectively collecting solid residues and filtrate, dialyzing the filtrate by using a semipermeable membrane to remove monosaccharide molecules, and mixing the obtained product with the solid residues to obtain a material to be detected;
b. taking the material to be tested, adding 100ml of water saturated n-butyl alcohol, heating and refluxing for 1 hour, filtering, washing the filtrate with ammonia test solution for 2 times, 50ml each time, discarding the ammonia washing solution, taking the n-butyl alcohol solution, washing with 50ml of water saturated with n-butyl alcohol, taking the n-butyl alcohol layer to dry, dissolving the residue with methanol 2 ml, filtering with a sample filter, and taking the subsequent filtrate as a test sample solution;
(2) Preparation of control solutions:
accurately weighing pseudoginsenoside F 11 The control 10.05 mg was placed in a 50ml volumetric flask and dissolved and diluted with methanolReleasing to scale, and shaking to obtain reference solution;
(3) Preparation of negative control solution:
taking a ginseng-lacking medicinal material, preparing a negative control sample according to a prescription process, weighing 18 g, and preparing a ginseng-lacking negative control solution by the same method as the preparation method of the test sample solution;
(4) The determination method comprises the following steps:
detecting by high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD), setting detection conditions, respectively sucking 15 μ L of each of the sample solution, the control solution and the negative control solution, and sampling for detection;
(5) And (5) judging a result:
in the chromatogram of the test sample, no chromatographic peak with the same retention time as that of the chromatographic peak of the reference sample should appear.
In step (4), the chromatographic conditions were the same as in example 1.
The preparation method of the semipermeable membrane in the step (1) comprises the following steps:
A. mixing alkaline basalt nano powder with 0.2 times of silicone oil, placing the mixture in a dispersion machine at 1500r/min for dispersion for 1.5h to obtain nano powder, and mixing the nano powder with 50 times of water to prepare dispersion liquid;
B. and (3) taking a certain amount of filter paper, immersing the filter paper in 75% cold sulfuric acid by using a glass rod, taking out the filter paper after immersing for 75s, spraying a saturated carbonic acid solution on the surface of the filter paper, wherein the spraying amount is 8%, putting the filter paper into the dispersion liquid obtained in the step A to rinse for 2 times after finishing spraying, putting the filter paper into dilute ammonia water to soak for 4min, taking out and drying to obtain the semipermeable membrane.
The filtering membrane of the sample filter in the step (1) is a modified regenerated cellulose filtering membrane, and the pore diameter of the modified regenerated cellulose filtering membrane is 0.35 mu m.
The preparation method of the modified regenerated cellulose filter membrane comprises the following steps:
s1, preparing a controlled release pore-forming agent: granulating the pore-forming agent for later use, dissolving poly N2 isopropyl acrylamide in deionized water at 25 ℃ to prepare a material liquid, spraying the obtained material liquid on the surface of the granulated pore-forming agent at 32 ℃ and 1.25MPa, heating to 45 ℃ and preserving heat for 25min to obtain the controlled-release pore-forming agent;
s2, preparing a membrane preparation liquid: dissolving cellulose in a solvent, then adding polylactic acid, a controlled-release pore-forming agent and an additive, uniformly mixing, defoaming and filtering to obtain a membrane-making solution;
s3, film making: and (2) casting the membrane-forming liquid prepared in the step (S2) on a glass plate to form a flat membrane at the temperature of 82 ℃, standing the flat membrane for 4S at the temperature of 45 ℃ in an aeration environment, stopping aeration, cooling the flat membrane to the temperature below 30 ℃, standing for 40min, standing for 8S in the aeration environment, putting the flat membrane into a coagulating bath, curing for 12min to form a membrane, washing away residual solvent in the membrane with deionized water, and airing at room temperature to obtain the modified regenerated cellulose filtering membrane.
In the step S1, the mass ratio of the material liquid to the pore-forming agent is 0.1:1, the mass concentration of poly N2 isopropyl acrylamide in the material liquid is 6 percent; in the step S2, the mass ratio of the cellulose to the polylactic acid to the controlled-release pore-forming agent to the additive is 1:0.45:0.22:0.03.
in the step S1, the pore-forming agent comprises a pore-forming agent A and a pore-forming agent B, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1:0.45, granulating the pore-forming agent A and the pore-forming agent B separately, wherein the pore-forming agent A is polyethylene glycol, the pore-forming agent B is sodium chloride and sodium alginate, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1:2.2.
the solvent in the step S2 is prepared from the following components in proportion of 3:1, the additive is polysorbate; the aeration environment in step S3 is: nitrogen gas with a ventilation of 0.08m 3 /h。
Example 8
The embodiment provides a method for detecting the components of American ginseng in Chinese and western ginseng pills, which comprises the following steps:
(1) Preparation of a test solution:
a. removing honey in the ginseng spleen-invigorating pills: taking 2 pills of ginseng spleen-invigorating pills, cutting into pieces, adding 50ml water, stirring for 12min at 42 ℃, then filtering, respectively collecting solid residues and filtrate, dialyzing the filtrate by using a semipermeable membrane to remove monosaccharide molecules, and mixing the obtained product with the solid residues to obtain a material to be detected;
b. taking the material to be tested, adding 100ml of water saturated n-butyl alcohol, heating and refluxing for 1 hour, filtering, washing the filtrate with ammonia test solution for 2 times, 50ml each time, discarding the ammonia washing solution, taking the n-butyl alcohol solution, washing with 50ml of water saturated with n-butyl alcohol, taking the n-butyl alcohol layer to dry, dissolving the residue with methanol 2 ml, filtering with a sample filter, and taking the subsequent filtrate as a test sample solution;
(2) Preparation of control solutions:
collecting pseudoginsenoside F 11 Precisely weighing a reference substance, adding methanol to prepare a solution containing 50 micrograms per 1ml, and shaking up to obtain the reference substance solution;
(3) Preparation of negative control solution:
taking a ginseng-lacking medicinal material, preparing a negative control sample according to a prescription process, weighing 18 g, and preparing a ginseng-lacking negative control solution by the same method as the preparation method of the test sample solution;
(4) The determination method comprises the following steps:
detecting by high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), setting detection conditions, respectively absorbing 15 μ L of test solution, control solution and negative control solution, and performing sample injection detection;
(5) And (5) judging a result:
in the chromatogram of the test sample, no chromatographic peak with the same retention time as that of the chromatographic peak of the reference sample should appear.
In step (4), the chromatographic conditions and mass spectrometric conditions were the same as in example 2.
The semipermeable membrane in the step (1) was prepared in the same manner as in example 7.
The filtration membrane of the sample filter in the step (1) was a modified regenerated cellulose filtration membrane having a pore size of 0.35 μm, and the preparation method thereof was the same as in example 7.
Application of detection method in controlling ginseng quality in ginseng spleen-invigorating pills
Selecting 10 batches of samples of ginseng spleen-invigorating pills (big honeyed pills) of which the batch numbers are removed by 2 production enterprises (enterprises A and B), respectively determining according to the detection methods of the embodiments 7 and 8, and judging whether the samples are detectedPseudo-ginseng saponin F 11 The results are shown in the following table:
TABLE 1
As can be seen from the results in Table 1, no pseudoginsenoside F was detected in 10 samples of ginseng spleen-invigorating pills from Enterprise A 11 The product is qualified; pseudo-ginsenoside F is detected in 10 batches of ginseng spleen-invigorating pill samples of B enterprise 11 The ginseng is suspected to be replaced by the leftover material of the American ginseng.
In order to judge the detection result in more detail and intuitively, the invention also provides a relevant map, which is shown in the attached figures 1 to 11.
As shown in figure 1, pseudoginsenoside F 11 The chromatogram of the reference substance shows a characteristic chromatographic peak; as shown in FIG. 2, in the chromatogram of the negative control sample, pseudoginsenoside F was not detected 11 。
As shown in FIG. 5, pseudoginsenoside F 11 The characteristic base peak is shown in the full-scanning base peak image of the reference substance; as shown in fig. 8, in the full-scan base peak pattern of the negative control sample, pseudoginsenoside F11 was not detected.
The invention adopts example 7 (HPLC-ELSD inspection method) to detect the sample of the batch No. 17013851 of the A enterprise, the chromatogram thereof is shown in figure 3, the chromatographic peak with the same retention time as the chromatographic peak of the reference substance in figure 1 does not appear in figure 3, and the invention proves that the sample of the batch No. 17013851 of the A enterprise does not detect the pseudoginsenoside F 11 。
The invention adopts the HPLC-MS/MS inspection method of example 8 to detect the sample of the batch No. 20170205 of the B enterprise, the chromatogram thereof is shown in figure 4, the chromatographic peak with the same retention time as the chromatographic peak of the reference substance in figure 1 appears in figure 4, and the pseudoginsenoside F detected by the sample of the batch No. 20170205 of the B enterprise is proved 11 (ii) a Then, the determination of pseudoginsenoside F was confirmed by mass spectrometry, as shown in FIGS. 9-11 11 。
The invention has the beneficial effects that: the invention provides a method for detecting the components of American ginseng and western ginseng in a ginseng-spleen-invigorating pill, which can effectively improve the accuracy and stability of sample detection through reasonable detection method and parameter design and complete sample pretreatment measures, is convenient to popularize and use, can be simultaneously used for detection by a high performance liquid chromatography-evaporative light scattering detector (HPLC-ELSD) detection method and a high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) detection method, and has strong applicability.
Finally, it should be noted that the above-mentioned embodiments are only preferred embodiments of the present invention, and not intended to limit the present invention, and although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications and equivalents can be made in the technical solutions described in the foregoing embodiments, or some technical features thereof can be replaced. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (3)
1. A detection method for Chinese and western ginseng components in a ginseng spleen-invigorating pill is characterized by comprising the following steps: the method comprises the following steps:
(1) Preparation of a test solution:
a. removing honey in the ginseng spleen-invigorating pills: taking 2 pills of ginseng spleen-invigorating pills, cutting into pieces, adding 50ml water, stirring for 10-15min at 40-45 ℃, then filtering, respectively collecting solid residues and filtrate, dialyzing the filtrate with a semipermeable membrane to remove monosaccharide molecules, and mixing the obtained product with the solid residues to obtain a material to be detected;
b. taking the material to be detected, adding 100ml of water saturated n-butyl alcohol, heating and refluxing for 1 hour, filtering, washing the filtrate with ammonia test solution for 2 times, 50ml each time, discarding the ammonia washing solution, taking the n-butyl alcohol solution, washing with 50ml of water saturated with n-butyl alcohol, taking the n-butyl alcohol layer to dry, dissolving the residue with methanol 2 ml, filtering with a sample filter, and taking the subsequent filtrate as a sample solution;
(2) Preparation of control solutions:
collecting pseudoginsenoside F 11 Accurately weighing reference substance, and adding methanol to obtain reference substance solution;
(3) Preparation of negative control solution:
taking a ginseng-lacking medicinal material, preparing a negative control sample according to a prescription process, weighing 18 g, and preparing a ginseng-lacking negative control solution by the same method as the preparation method of the test sample solution;
(4) The determination method comprises the following steps:
detecting by high performance liquid chromatography-evaporative light scattering detector detection method or high performance liquid chromatography-tandem mass spectrometry detection method, setting detection conditions, respectively sucking 10-20 μ L of sample solution, reference solution, and negative reference solution, and performing sample injection detection;
(5) And (5) judging a result:
in the chromatogram of the test sample, a chromatographic peak with the same retention time as that of the chromatographic peak of the reference sample cannot appear;
the preparation method of the semipermeable membrane in the step (1) comprises the following steps:
A. mixing the alkaline basalt nano powder with 0.1-0.3 times of silicone oil, placing the mixture in a dispersion machine of 1000-2000r/min for dispersing for 1-2h to obtain nano powder, and mixing the nano powder with 40-60 times of water to prepare dispersion liquid;
B. taking a certain amount of filter paper, immersing the filter paper in 75% cold sulfuric acid by using a glass rod, taking out the filter paper after soaking for 70-80s, spraying a saturated carbonic acid solution on the surface of the filter paper, wherein the spraying amount is 6-10%, putting the filter paper into the dispersion liquid obtained in the step A after spraying is finished, rinsing for 1-3 times, putting the filter paper into dilute ammonia water, soaking for 3-5min, taking out and airing to obtain a semipermeable membrane;
the filtering membrane of the sample filter in the step (1) is a modified regenerated cellulose filtering membrane, and the aperture of the modified regenerated cellulose filtering membrane is 0.2-0.5 mu m;
the preparation method of the modified regenerated cellulose filter membrane comprises the following steps:
s1, preparing a controlled release pore-forming agent: granulating the pore-forming agent for later use, dissolving poly (N-isopropylacrylamide) in deionized water at 24-26 ℃ to prepare a material liquid, spraying the obtained material liquid on the surface of the granulated pore-forming agent at 31-33 ℃ and 1-1.5MPa, then heating to 40-50 ℃ and preserving heat for 20-30min to obtain the controlled-release pore-forming agent;
s2, preparing a membrane preparation liquid: dissolving cellulose in a solvent, then adding polylactic acid, a controlled-release pore-forming agent and an additive, uniformly mixing, defoaming and filtering to obtain a membrane-making solution;
s3, film making: casting the membrane-forming solution prepared in the step S2 on a glass plate at the temperature of 80-84 ℃ to form a flat membrane, standing the flat membrane for 3-5S at the temperature of 40-50 ℃ in an aeration environment, stopping aeration, cooling the flat membrane to below 30 ℃, standing for 30-50min, standing for 5-10S in the aeration environment, putting the flat membrane into a coagulating bath, curing for 10-15min to form a membrane, washing away residual solvent in the membrane by using deionized water, and airing at room temperature to obtain the modified regenerated cellulose filtering membrane;
in the step S1, the mass ratio of the material liquid to the pore-forming agent is (0.08-0.12): 1, the mass concentration of poly (N-isopropyl acrylamide) in the material liquid is 4-8%; in the step S2, the mass ratio of the cellulose to the polylactic acid to the controlled-release pore-forming agent to the additive is 1: (0.3-0.6): (0.15-0.3): (0.02-0.05);
in the step S1, the pore-forming agent comprises a pore-forming agent A and a pore-forming agent B, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1: (0.3-0.6), separately granulating the pore-forming agent A and the pore-forming agent B, wherein the pore-forming agent A is polyethylene glycol, the pore-forming agent B is sodium chloride and sodium alginate, and the mass ratio of the pore-forming agent A to the pore-forming agent B is 1: (1.5-3);
the solvent in the step S2 is (2-4): 1, dimethyl sulfoxide/tetraethyl ammonium chloride, and the additive is fatty glyceride or polysorbate; the aeration environment in step S3 is: nitrogen or argon with a ventilation of 0.05-0.1m 3 /h。
2. The method for detecting the American ginseng components in the ginseng spleen-invigorating pill according to claim 1, which is characterized in that:
and (4) detecting by adopting a high performance liquid chromatography-evaporative light scattering detector inspection method, wherein the chromatographic conditions are as follows: a chromatographic column: capcell pak C18,4.6 mm. Times.250mm, 5 μm, mobile phase: acetonitrile-water, volume ratio 30; evaporative light scattering detector: gas flow rate: 1.6 L/min, flow rate: 1ml/min, and the column temperature is 30 ℃;
in this case, the preparation method of the reference solution in the step (2) is as follows: accurately weighing pseudoginsenoside F 11 And (3) placing a reference substance 10.05 mg in a 50ml measuring flask, adding methanol to dissolve and dilute the solution to a scale, and shaking the solution uniformly to obtain a reference substance solution.
3. The method for detecting the American ginseng components in the ginseng spleen-invigorating pill according to claim 1, which is characterized in that:
and (4) detecting by adopting a high performance liquid chromatography-tandem mass spectrometry inspection method, wherein the chromatographic conditions are as follows:
chromatographic column Waters ACQUITY UPLC BEH-C 18 2.1mm × 100mm,1.7 μm; acetonitrile is taken as a mobile phase A, and water is taken as a mobile phase B; the flow rate is 0.4 ml/min; the column temperature is 40 ℃; 3 mu L of sample volume;
gradient elution: 0-12 min, 8-80% A; for 12-14 min, 80-90% of A; 14-14.2 min,90% -8% of A; 14.2-20 min,8% A; the volume ratio of acetonitrile to water is 30;
the mass spectrum conditions are as follows: taking a flight time mass spectrum as a detector, adopting an electrospray ionization ion source and a negative ion mode for detection, taking Leucine-enkephalin as a calibration solution, and scanning the range: m/z is 50-1200, the sampling interval is 0.5s, the capillary voltage is 2.5kV, the taper hole voltage is 40V, the ion source temperature is 100 ℃, the desolvation temperature is 450 ℃, and the desolvation gas flow rate is 800 L.h -1 Cone hole gas flow rate of 40 L.h -1 The collision gas is argon; the collision low energy is 6V, and the collision high energy is 20-40V;
in this case, the preparation method of the reference solution in the step (2) is as follows: collecting pseudoginsenoside F 11 And (3) precisely weighing a reference substance, adding methanol to prepare a solution containing 50 microgram per 1ml, and shaking up to obtain the reference substance solution.
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