A method and system for analyzing the hi value of a liquid soy phospholipid product

Abstract

The application discloses a method and system for analyzing the HI value of a liquid soybean phospholipid product, and the method comprises the following steps: obtaining an ultrasonic-dissolved liquid soybean phospholipid sample, centrifuging the liquid soybean phospholipid sample by using an ultracentrifuge, repeatedly performing centrifugal precipitation operation on the precipitate for 2-3 times, obtaining sample residues, vacuum drying the sample residues, and calculating the hexane-insoluble content (HI) value in the sample residues after the drying is completed. By using the ultracentrifugation method, impurity particles in the phospholipid, especially small and tiny particles, can be quickly and completely precipitated in a short time, the HI value of the phospholipid can be accurately determined, the error of the analysis result is greatly reduced, and the data accuracy is improved. By repeatedly performing centrifugal precipitation operation on the precipitate for 2-3 times, the screening and omission of small-particle impurities can be more accurately ensured, and the stability of the test result is further ensured.

Description

TECHNICAL FIELD

[0001] The present application relates to the technical field of high-grade health care products and pharmaceutical-grade phospholipids, and particularly relates to a method and system for analyzing the HI value of a liquid soybean phospholipid product. BACKGROUND

[0002] Phospholipids are an important component of living cells, can promote human fat metabolism, reduce cholesterol, protect the liver, improve blood circulation, and prevent cardiovascular diseases. The United Nations Food and Agriculture Organization and the World Health Organization have approved it as one of the three major nutrients together with protein and vitamins. Therefore, soybean phospholipids are widely used in the health care and pharmaceutical industries and are known as the "garbage collector of blood vessels", "protector of cells", and "power to open the brain".

[0003] However, as a capsule health care product and pharmaceutical phospholipid, the raw material is very important. At present, the raw materials on the market are mixed, the quality is unstable, and the appearance is turbid and opaque. The reason is that some particulate impurities such as rust, soil, dust, chaff, protein, and sugar ester are brought into the soybean raw material in the production process of concentrated phospholipids, which affects the transparency and quality of the phospholipids. The main index of impurities is hexane insolubles, and the current national standard requires <0.3%. If these concentrated phospholipids are used as starting materials to produce powder phospholipids and food, health care products, and pharmaceutical deep processing, the quality will be unqualified due to excessive impurities. Imagine that there are 1-3 kg of black impurities in every ton of product, which will definitely bring unhygienic and unsafe hidden dangers to the product. Especially in the production of soybean phospholipids for injection, very small amounts of impurities in the raw material can cause heat source reaction in the human body, causing fever in patients, and in severe cases, coma and even life-threatening. The existing impurity filtering method adopts a G3 (pore size 16-30 pm) crucible filtering method, which is only suitable for filtering large-diameter impurities. Small particles and micro-particles leak into the solution through the pore size, causing HI analysis to be low and the analysis result to be inaccurate. SUMMARY

[0004] In view of the above problems, the present application provides a method and system for analyzing the HI value of a liquid soybean phospholipid product to solve the problem that the existing technology is only suitable for filtering large-diameter impurities, small particles and micro-particles leak into the solution through the pore size, causing HI analysis to be low and the analysis result to be inaccurate.

[0005] A method for analyzing the HI value of a liquid soybean phospholipid product, comprising the following steps:

[0006] Obtaining a liquid soybean phospholipid sample dissolved by ultrasonic waves;

[0007] Using an ultracentrifuge to centrifuge and precipitate the liquid soybean phospholipid sample;

[0008] The precipitate is subjected to repeated centrifugal precipitation operation 2-3 times to obtain sample residue;

[0009] The sample residue is vacuum dried, and after drying, the content (HI) of hexane-insoluble substances in the sample residue is calculated.

[0010] Preferably, the ultrasonic dissolved liquid soybean phospholipid sample is obtained by:

[0011] 5-10g of soybean phospholipid sample is weighed into a centrifuge tube;

[0012] According to the first proportion, n-hexane is added to the centrifuge tube for dissolution;

[0013] The real-time dissolution efficiency during the dissolution process is detected;

[0014] If the real-time dissolution efficiency is greater than or equal to the preset threshold value, no subsequent operation is needed, otherwise, auxiliary dissolution is performed using ultrasonic waves to obtain an ultrasonic dissolved liquid soybean phospholipid sample.

[0015] Preferably, the liquid soybean phospholipid sample is subjected to centrifugal precipitation using an ultracentrifuge to obtain supernatant and precipitate, including:

[0016] The separation factor, centrifugal force, centrifugal time and centrifugal temperature of the ultracentrifuge are set;

[0017] After setting, the centrifuge tube is sealed using the centrifuge tube rotor cover of the ultracentrifuge;

[0018] The ultracentrifuge is started to centrifuge the mixture of soybean phospholipid sample and n-hexane in the centrifuge tube to obtain supernatant and precipitate.

[0019] Preferably, the centrifuge tube rotor cover of the ultracentrifuge adopts a double locking structure.

[0020] Preferably, the separation factor of the ultracentrifuge is determined by the following method:

[0021] The factory parameters of the ultracentrifuge are obtained;

[0022] The drum radius and the running speed range of the drum of the ultracentrifuge are determined according to the factory parameters;

[0023] The separation factor setting range of the ultracentrifuge is calculated according to the drum radius and the running speed range of the drum of the ultracentrifuge:

[0024] ;

[0025] Wherein, represents the minimum separation factor or the maximum separation factor of the ultracentrifuge, represents the circle ratio, and takes the value of 3.14, r represents the radius of the bowl of the ultracentrifuge, represents the minimum rotational speed or the maximum rotational speed in the operating rotational speed interval of the bowl of the ultracentrifuge, g represents the acceleration of gravity;

[0026] In the separation factor setting interval of the ultracentrifuge, a target separation factor greater than or equal to 15000G is selected as the setting separation factor of the ultracentrifuge.

[0027] Preferably, the centrifugal force of the ultracentrifuge is determined by the following method:

[0028] The densities of the particles and the solution in the mixture of the soybean phospholipid sample and n-hexane and the viscosity of the solution are detected;

[0029] The settling speed of the soybean phospholipid sample in the n-hexane is calculated according to the densities of the particles and the solution in the mixture of the soybean phospholipid sample and n-hexane and the viscosity of the solution:

[0030] ;

[0031] wherein, represents the settling speed of the soybean phospholipid sample in the n-hexane, represents the particle density in the mixture of the soybean phospholipid sample and n-hexane, represents the solution density in the mixture of the soybean phospholipid sample and n-hexane, d represents the maximum particle diameter in the mixture of the soybean phospholipid sample and n-hexane, represents the solution viscosity in the mixture of the soybean phospholipid sample and n-hexane;

[0032] According to the settling speed of the soybean phospholipid sample in the n-hexane, a corresponding target centrifugal force is selected as the setting centrifugal force of the ultracentrifuge.

[0033] Preferably, the precipitate is subjected to repeated centrifugal precipitation operation 2-3 times to obtain a sample residue, including:

[0034] According to the second proportion, n-hexane is added in the centrifugal tube to perform repeated centrifugal precipitation operation 2-3 times to obtain a sample residue.

[0035] Preferably, the sample residue is subjected to vacuum drying, and after the drying is completed, the hexane insoluble content (HI) value in the sample residue is calculated, including:

[0036] The vacuum drying temperature and the drying time are set;

[0037] vacuum drying the sample residue according to the vacuum drying temperature and the drying duration until the sample residue meets a determination condition that the sample residue maintains a constant weight during the vacuum drying process;

[0038] obtaining a sample mass and a centrifuge tube mass of the soybean phospholipid sample and a total mass of the centrifuge tube and the sample residue after vacuum drying;

[0039] calculating a hexane insoluble content (HI) ratio of the soybean phospholipid sample according to the sample mass and the centrifuge tube mass of the soybean phospholipid sample and the total mass of the centrifuge tube and the sample residue after vacuum drying;

[0040]

[0041] wherein X represents the hexane insoluble content (HI) ratio of the soybean phospholipid sample, represents the total mass of the centrifuge tube and the sample residue after vacuum drying, represents the centrifuge tube mass, represents the sample mass of the soybean phospholipid sample.

[0042] Preferably, before weighing 5-10 g of the soybean phospholipid sample into the centrifuge tube, the method further comprises:

[0043] performing mapping on the weighed soybean phospholipid sample to obtain a surface morphology thereof;

[0044] constructing a three-dimensional model of the soybean phospholipid sample according to the surface morphology and mapping parameters;

[0045] performing mesh scanning on the three-dimensional model, and determining whether the soybean phospholipid sample is hollow according to a scanning result, if yes, confirming that it does not meet the test requirements, otherwise, preliminarily confirming that it meets the test requirements;

[0046] immersing the soybean phospholipid sample in clean water for a target duration, performing component analysis on the soaked clean water, and obtaining an analysis result;

[0047] determining sensitive parameters in the soybean phospholipid sample according to the analysis result;

[0048] testing an influence value of each sensitive parameter on the n-hexane solubility;

[0049] constructing a n-hexane solubility degradation trajectory model under the sensitive parameters according to the influence value;

[0050] calculating an error factor of the final HI value through the solubility degradation trajectory model;

[0051] evaluating whether the soybean phospholipid sample is qualified according to the error factor, if yes, taking it as a test sample, otherwise, reselecting the soybean phospholipid sample to repeat the above test until passing the test.​

[0052] A system for analyzing the HI value of liquid soybean lecithin products, the system comprising:

[0053] The first acquisition module is used to acquire liquid soybean lecithin samples dissolved by ultrasonication;

[0054] A precipitation module is used to centrifuge and precipitate the liquid soybean lecithin sample using an ultracentrifuge.

[0055] The second acquisition module is used to perform repeated centrifugation and precipitation operations on the precipitate 2-3 times to obtain sample residue;

[0056] The calculation module is used to perform vacuum drying on the sample residue, and after drying, calculate the hexane insoluble content (HI) value in the sample residue.

[0057] Other features and advantages of the invention will be set forth in the following description, and will be apparent in part from the description, or may be learned by practicing the invention. The objects and other advantages of the invention may be realized and obtained by means of the structures particularly pointed out in the written description and the accompanying drawings.

[0058] The technical solution of the present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Attached Figure Description

[0059] The accompanying drawings are provided to further illustrate the invention and form part of the specification. They are used together with the embodiments of the invention to explain the invention and do not constitute a limitation thereof.

[0060] Figure 1 A flowchart illustrating the process of a method for analyzing the HI value of liquid soybean lecithin products provided by this invention;

[0061] Figure 2 Another flowchart of a method for analyzing the HI value of liquid soybean lecithin products provided by the present invention;

[0062] Figure 3 Screenshot of an embodiment of a method for analyzing the HI value of liquid soybean lecithin products according to the present invention;

[0063] Figure 4 This is a schematic diagram of the structure of a system for analyzing the HI value of liquid soybean lecithin products provided by the present invention. Detailed Implementation

[0064] The exemplary embodiments will be described in detail herein with reference to examples thereof as illustrated in the accompanying drawings. The following description is presented in the context of the drawings, where like numbers represent like or similar elements for the same or similar elements shown throughout the several figures of the drawing. The implementations described in the following exemplary embodiments do not represent all implementations consistent with the present disclosure. Instead, they are merely examples of apparatuses and methods consistent with some aspects of the present disclosure as detailed in the appended claims.

[0065] Phospholipids are an important component of living cells, can promote human fat metabolism, reduce cholesterol, protect the liver, improve blood circulation, prevent cardiovascular disease. Has been approved by the Food and Agriculture Organization of the United Nations and the World Health Organization as one of the three nutrients together with protein, vitamins. So the soybean phospholipid is widely used in health care products and pharmaceutical industry, known as "the scavenger of blood vessels", "the protector of cells", "the power to open the brain".

[0066] But as a capsule health care products and pharmaceutical phospholipids, the raw material is very important, the current market raw materials mixed, unstable quality, appearance turbidity opaque, the reason is that the production process of concentrated phospholipids, soybean raw materials will bring some granular impurities, such as rust, soil, dust, bran, protein, sugar ester, etc., affect the transparency and quality of phospholipids. The main index of impurities is hexane insoluble, the current national standard requires <0.3%, if these concentrated phospholipids as starting material to make powder phospholipid and food, health care products and pharmaceutical deep processing, will lead to unqualified quality due to impurities, imagine every ton of product 1-3 kg of black unclean material exists, will bring unhygienic, unsafe hidden trouble. Especially in the production of soybean phospholipid for injection, very small amount of impurities in the raw material may cause the body to produce heat source reaction, leading to fever in patients, severe coma and even endanger life. The existing impurity filtration method adopts G3 (pore size 16-30 μm) crucible filtration method, which is only suitable for filtering large diameter impurities. Small particles and micro particles leak into the solution through the pore size, resulting in low HI analysis and inaccurate analysis results. In order to solve the above problems, the embodiment discloses a method for analyzing the HI value of liquid soybean phospholipid product.

[0067] A method for analyzing the HI value of liquid soybean phospholipid product, as shown in Figure 1 , comprising the following steps:

[0068] Step S101, obtaining an ultrasonic dissolved liquid soybean phospholipid sample;

[0069] Step S102, using an ultracentrifuge to centrifuge and precipitate the liquid soybean phospholipid sample;

[0070] Step S103, repeating the centrifugation and precipitation operation 2-3 times to obtain sample residue;

[0071] Step S104, vacuum drying the sample residue, and calculating the hexane insoluble content (HI) value in the sample residue after drying.

[0072] The working principle of the technical solution is as follows: liquid soybean phospholipid samples dissolved by ultrasonic waves are obtained, the liquid soybean phospholipid samples are centrifuged by using an ultracentrifuge, the precipitate is subjected to repeated centrifugal precipitation operation 2-3 times, sample residue is obtained, and the sample residue is vacuum dried, and the hexane insoluble content (HI) value in the sample residue is calculated after drying.

[0073] The beneficial effects of the technical solution are as follows: by using the ultracentrifugation method, impurity particles in the phospholipid, especially small particles, can be quickly and completely precipitated in a short time, the HI value of the phospholipid can be accurately measured, the error of the analysis result is greatly reduced, the accuracy of the data is improved, further, the repeated centrifugal precipitation operation 2-3 times on the precipitate can more accurately ensure the screening and omission of small particle impurities, further ensure the stability of the test result, solve the problem that only large-diameter impurities are filtered in the prior art, small particles and micro particles leak into the solution through the pore size, causing the HI analysis to be low and the analysis result to be inaccurate, lay a foundation for manufacturers to quickly and efficiently select high-quality phospholipid raw materials when selecting raw materials, and improve the user experience.

[0074] In one embodiment, as shown in Figure 2 The ultrasonic wave dissolved liquid soybean phospholipid sample is obtained by:

[0075] Step S201, weighing 5-10g of soybean phospholipid sample into a centrifuge tube;

[0076] Step S202, adding n-hexane for dissolution according to a first ratio in the centrifuge tube;

[0077] Step S203, detecting the real-time dissolution efficiency in the dissolution process;

[0078] Step S204, confirming whether the real-time dissolution efficiency is greater than or equal to a preset threshold value, if yes, no subsequent operation is needed, otherwise, auxiliary dissolution is performed by using ultrasonic waves to obtain the liquid soybean phospholipid sample dissolved by ultrasonic waves.

[0079] In the embodiment, the first ratio is represented as the ratio of the soybean phospholipid sample and n-hexane, and the ratio can be 1:2-10 (m / v).

[0080] The beneficial effects of the above technical solutions are: the use of ultrasonic waves for auxiliary dissolution can further accelerate the dissolution speed, improve the dissolution efficiency, ensure complete dissolution of the sample, and improve the stability.

[0081] In one embodiment, the liquid soybean phospholipid sample is centrifuged by using an ultracentrifuge to obtain supernatant and precipitate, comprising:

[0082] The separation factor, centrifugal force, centrifugation time and centrifugation temperature of the ultracentrifuge are set;

[0083] After setting, the centrifuge tube is sealed by using the centrifuge tube rotor cover of the ultracentrifuge;

[0084] The mixture of soybean phospholipid sample and n-hexane in the centrifuge tube is centrifuged by starting the ultracentrifuge to obtain supernatant and precipitate;

[0085] In this embodiment, the centrifugation time can be 5-30 min, preferably 5-10 min, the centrifugation temperature can be 0-20 degrees, and the separation factor is ≥15000g. With the increase of the separation factor of the centrifuge, the HI value of the same sample also gradually increases. Through a large number of HI condition experiments, we found that when the separation factor is greater than 15000g, the HI value tends to be stable, and the HI result is basically the same as that obtained by using an ultracentrifuge with a separation factor greater than 500,000g. Therefore, the separation factor of the centrifuge must be ≥15000g.

[0086] The beneficial effects of the above technical solutions are: by setting the working parameters of the ultracentrifuge, the mixture of soybean phospholipid sample and n-hexane in the centrifuge tube can be quickly and stably centrifuged, further improving the work efficiency. Further, by sealing the centrifuge tube by using the centrifuge tube rotor cover of the ultracentrifuge, the calculation error caused by the water absorption property of phospholipids can be avoided, and the data accuracy is further ensured.

[0087] In one embodiment, the centrifuge tube rotor cover of the ultracentrifuge adopts a double locking structure.

[0088] The beneficial effects of the above technical solutions are: the inaccuracy of the results caused by water absorption of phospholipids during centrifugation can be avoided, the practicability is improved, and the stability is further improved.

[0089] In one embodiment, the separation factor of the ultracentrifuge is determined by the following method:

[0090] The factory parameters of the ultracentrifuge are obtained;

[0091] The drum radius and the running speed range of the drum of the ultracentrifuge are determined according to the factory parameters.

[0092] According to the radius of the rotating drum of the ultracentrifuge and the operation speed interval of the rotating drum, a separation factor setting interval of the ultracentrifuge is calculated:

[0093] ;

[0094] wherein, represents the minimum separation factor or the maximum separation factor of the ultracentrifuge, represents the circular constant, and is 3.14, and r represents the radius of the rotating drum of the ultracentrifuge, represents the minimum speed or the maximum speed in the operation speed interval of the rotating drum of the ultracentrifuge, and g represents the acceleration of gravity;

[0095] A target separation factor greater than or equal to 15000G is selected as the setting separation factor of the ultracentrifuge in the separation factor setting interval of the ultracentrifuge.

[0096] The technical scheme has the beneficial effects that the separation factor setting interval of the ultracentrifuge is calculated to provide a selection space for the staff, and the separation factor of the ultracentrifuge is intelligently selected according to the actual use demand, thereby further improving the practicability.

[0097] In an embodiment, the centrifugal force of the ultracentrifuge is determined by the following method:

[0098] The densities of the particles and the solution in the mixture of the soybean phospholipid sample and n-hexane and the viscosity of the solution are detected;

[0099] The settling speed of the soybean phospholipid sample in the n-hexane is calculated according to the densities of the particles and the solution in the mixture of the soybean phospholipid sample and n-hexane and the viscosity of the solution:

[0100] ;

[0101] wherein, represents the settling speed of the soybean phospholipid sample in the n-hexane, represents the particle density in the mixture of the soybean phospholipid sample and n-hexane, represents the solution density in the mixture of the soybean phospholipid sample and n-hexane, and d represents the maximum particle diameter in the mixture of the soybean phospholipid sample and n-hexane, represents the solution viscosity in the mixture of the soybean phospholipid sample and n-hexane;

[0102] A corresponding target centrifugal force is selected as the setting centrifugal force of the ultracentrifuge according to the settling speed of the soybean phospholipid sample in the n-hexane.

[0103] The beneficial effects of the above technical solutions are: the centrifugal force is selected according to the settling speed of the soybean phospholipid sample in the n-hexane, the required centrifugal force can be evaluated according to the natural dissolution of the sample, the dissolution rate of the sample is accelerated while the sample is not excessively dissolved under the strong traction of the centrifugal force, and the practicability is further improved.

[0104] In one embodiment, the precipitate is subjected to repeated centrifugal precipitation operation 2-3 times to obtain a sample residue, including:

[0105] According to the second ratio, n-hexane is added to the centrifugal tube for repeated centrifugal precipitation operation 2-3 times to obtain a sample residue;

[0106] In this embodiment, the above-mentioned second ratio can be 1:2-5 (m / v), preferably 1:2-3 (m / v).

[0107] The beneficial effects of the above technical solutions are: the excessive loss of n-hexane can be saved, and the precipitate can be cleaned, further improving the practicability.

[0108] In one embodiment, the sample residue is subjected to vacuum drying, and after drying, the hexane-insoluble content (HI) value of the sample residue is calculated, including:

[0109] The vacuum drying temperature and drying time are set;

[0110] The sample residue is vacuum dried according to the vacuum drying temperature and drying time until it meets the determination condition, and the determination condition is that the sample residue maintains a constant weight during vacuum drying;

[0111] The sample mass of the soybean phospholipid sample and the centrifugal tube mass and the total mass of the centrifugal tube and the vacuum-dried sample residue are obtained;

[0112] The hexane-insoluble content (HI) ratio of the soybean phospholipid sample is calculated according to the sample mass of the soybean phospholipid sample and the centrifugal tube mass and the total mass of the centrifugal tube and the vacuum-dried sample residue:

[0113] ;

[0114] Wherein, X represents the hexane-insoluble content (HI) ratio of the soybean phospholipid sample, represents the total mass of the centrifugal tube and the vacuum-dried sample residue, represents the centrifugal tube mass, represents the sample mass of the soybean phospholipid sample;

[0115] In this embodiment, the drying temperature can be 50 degrees, the vacuum degree reaches-0.098 MPa, and the drying time can be 20-60 min.

[0116] The technical scheme has the beneficial effects that the rationality of the sample residue used for calculation is ensured, and objective and accurate data are calculated.

[0117] In one embodiment, before the soybean phospholipid sample is weighed 5-10 g into the centrifuge tube, the method further comprises:

[0118] The weighed soybean phospholipid sample is profiled to obtain a surface morphology thereof;

[0119] A three-dimensional model of the soybean phospholipid sample is constructed according to the surface morphology and the profiling parameters;

[0120] The three-dimensional model is subjected to mesh scanning, and it is determined according to the scanning result whether the soybean phospholipid sample is hollow inside, if yes, it is confirmed that the sample does not meet the test requirements, otherwise, it is preliminarily confirmed that the sample meets the test requirements;

[0121] The soybean phospholipid sample is placed in clean water for a target time length, and the composition of the soaked clean water is analyzed to obtain an analysis result;

[0122] Sensitive parameters in the soybean phospholipid sample are determined according to the analysis result;

[0123] The influence value of each sensitive parameter on the n-hexane dissolution rate is tested;

[0124] A dissolution degradation trajectory model of n-hexane under the sensitive parameters is constructed according to the influence value;

[0125] An error factor of the final HI value is calculated through the dissolution degradation trajectory model;

[0126] It is determined according to the error factor whether the soybean phospholipid sample is qualified, if yes, the sample is used as a test sample, otherwise, the soybean phospholipid sample is reselected and the above test is repeated until the test is passed.

[0127] The technical scheme has the beneficial effects that whether the soybean phospholipid sample meets the test requirements can be comprehensively evaluated, the situation that the calculation result is greatly inconsistent with the actual situation due to the change of the composition of the soybean phospholipid sample caused by long storage time of the sample is avoided, and the stability and practicality are further improved.

[0128] In one embodiment, as Figure 3 shown, the present application is implemented by the following technical scheme:

[0129] (1) Weighing the sample: weighing 5-10 g of the sample into a weighed centrifuge tube, adding n-hexane to dissolve the solution, and ultrasonic dissolution;

[0130] (2) Ultra-centrifuge centrifugal precipitation: centrifugal precipitation in a sealed centrifuge tube at room temperature, to obtain supernatant and precipitate;

[0131] (3) Washing centrifugation: pour out the supernatant, and add n-hexane to the precipitate for washing cycle (2);

[0132] (4) Precipitate drying: pour out the supernatant, and place the centrifuge tube and the precipitate into an oven for vacuum drying, constant weight, and calculation;

[0133] Specific embodiment 1: Concentrate 10 g (accurate to 0.0001 g) of a phospholipid sample in a weighed centrifuge tube, add 80 ml of n-hexane, and ultrasonicate for 2 min for dissolution. Use an Avanti J-E high-performance centrifuge at a speed of 10,000 rpm, a separation factor of 15,300, and a centrifugation time of 5 min. Seal the centrifuge tube to ensure that n-hexane does not evaporate and does not absorb moisture in the air during high-speed centrifugation. Pour out the supernatant, add 40 ml of n-hexane to the precipitate, centrifuge for 5 min, ultrasonicate for dissolution, repeat three times, pour out the supernatant, and dry the centrifuge tube and insoluble impurities in an oven to constant weight. Calculate the content of n-hexane insolubles to be 0.006%.

[0134] Specific embodiment 2: Concentrate 10 g (accurate to 0.0001 g) of a phospholipid sample in a weighed centrifuge tube, add 80 ml of n-hexane, and ultrasonicate for 2 min for dissolution. Use an Avanti J-E high-performance centrifuge at a speed of 11,500 rpm, a separation factor of 20,000, and a centrifugation time of 5 min. Seal the centrifuge tube to ensure that n-hexane does not evaporate and does not absorb moisture in the air during high-speed centrifugation. Pour out the supernatant, add 40 ml of n-hexane to the precipitate, centrifuge for 5 min, ultrasonicate for dissolution, repeat three times, pour out the supernatant, and dry the centrifuge tube and insoluble impurities in an oven to constant weight. Calculate the content of n-hexane insolubles to be 0.0063%.

[0135] Specific embodiment 3: Concentrate 10 g (accurate to 0.0001 g) of a phospholipid sample in a weighed centrifuge tube, add 40 ml of n-hexane, and ultrasonicate for 2 min for dissolution. Use an Optima MAX-XP ultra-centrifuge at a speed of 105,000 rpm, a separation factor of 500,000, and a centrifugation time of 5 min. Seal the centrifuge tube to ensure that n-hexane does not evaporate and does not absorb moisture in the air during high-speed centrifugation. Pour out the supernatant, add 50 ml of n-hexane to the precipitate, centrifuge for 5 min, ultrasonicate for dissolution, repeat three times, pour out the supernatant, and dry the centrifuge tube and insoluble impurities in an oven to constant weight. Calculate the content of n-hexane insolubles to be 0.0065%.

[0136] By the technical scheme, sufficient precipitation and dissolution of fine particles relative to the filtering method of the crucible can be realized. Since the conventional low-speed centrifuge, the separation factor is generally below 4000, and since the separation factor is too low, the tiny impurities cannot precipitate quickly, and cannot completely precipitate. In addition, the boiling point of diethyl ether is relatively low, which is very unsafe. The national standard has been changed to hexane insoluble matter since 2012. The polarity of diethyl ether is greater than that of n-hexane, and the measured result is inherently lower than that of hexane insoluble matter, so it cannot be used. In addition, the centrifugation time is too long (which leads to solvent evaporation and phospholipid water absorption, so that the result is inaccurate, which has great limitations, and the measurement result error is large, so the technical scheme can effectively avoid the above situation, reduce the error of the measurement result, and make the final test result more accurate.

[0137] The embodiment also discloses a system for analyzing the HI value of a liquid soybean phospholipid product, as shown in the accompanying drawings, the system comprises: Figure 4

[0138] A first acquisition module 401 is configured to acquire a liquid soybean phospholipid sample dissolved by ultrasonic waves.

[0139] A precipitation module 402 is configured to perform centrifugal precipitation on the liquid soybean phospholipid sample by using an ultracentrifuge.

[0140] A second acquisition module 403 is configured to perform repeated centrifugal precipitation operation on the precipitate for 2-3 times, and acquire sample residues.

[0141] A calculation module 404 is configured to perform vacuum drying on the sample residues, and calculate the content (HI) value of hexane insoluble matter in the sample residues after the drying is completed.

[0142] The working principle and beneficial effects of the above technical scheme have been described in the method claim, and will not be repeated here.

[0143] Those skilled in the art should understand that the first and second in the present application refer to different application stages.

[0144] Other embodiments of the present disclosure will be readily apparent to those skilled in the art upon considering the specification and practicing the disclosure disclosed herein. The present application is intended to cover any variations, uses, or adaptive changes of the present disclosure that follow the general principles of the present disclosure and include common knowledge or conventional technical means in the technical field of the present disclosure not disclosed by the present disclosure. The specification and examples are only considered as exemplary, and the true scope and spirit of the present disclosure are indicated by the following claims.

[0145] It should be understood that the present disclosure is not limited to the precise structures already described and shown in the drawings, and various modifications and changes can be made without departing from the scope thereof. The scope of the present disclosure is limited only by the appended claims.​

Claims

1. A method of analyzing the HI value of a liquid soybean phospholipid product, characterized by, The method comprises the following steps: obtaining an ultrasonic dissolved liquid soybean phospholipid sample; using an ultracentrifuge to centrifugally precipitate the liquid soybean phospholipid sample; repeating the centrifugal precipitation operation on the precipitate for 2-3 times to obtain a sample residue; vacuum drying the sample residue, and calculating the hexane insoluble content (HI) value in the sample residue after drying; the method for obtaining the ultrasonic dissolved liquid soybean phospholipid sample comprises: weighing 5-10 g of the soybean phospholipid sample into a centrifuge tube; adding n-hexane for dissolution according to a first proportion in the centrifuge tube; detecting the real-time dissolution efficiency in the dissolution process; determining whether the real-time dissolution efficiency is greater than or equal to a preset threshold value, if yes, no subsequent operation is needed, otherwise, auxiliary dissolution is performed by using ultrasonic waves to obtain the ultrasonic dissolved liquid soybean phospholipid sample; using an ultracentrifuge to centrifugally precipitate the liquid soybean phospholipid sample, and obtaining supernatant and precipitate, comprising: setting the separation factor, centrifugal force, centrifugal time and centrifugal temperature of the ultracentrifuge; after the setting, sealing the centrifuge tube by using the centrifuge tube rotor cover of the ultracentrifuge; starting the ultracentrifuge to centrifugally precipitate the mixture of the soybean phospholipid sample and n-hexane in the centrifuge tube, and obtaining the supernatant and the precipitate; the separation factor of the ultracentrifuge is determined by the following method: obtaining the factory parameters of the ultracentrifuge; determining the drum radius and the running speed interval of the drum of the ultracentrifuge according to the factory parameters; calculating the separation factor setting interval of the ultracentrifuge according to the drum radius and the running speed interval of the drum of the ultracentrifuge: ； wherein represents the minimum separation factor or the maximum separation factor of the ultracentrifuge, represents the circle constant with a value of 3.14, and r represents the radius of the bowl of the ultracentrifuge, represents the minimum or maximum rotational speed in the operating rotational speed interval of the bowl of the ultracentrifuge, and g represents the acceleration due to gravity; selecting a target separation factor greater than or equal to 15000G in the separation factor setting interval of the ultracentrifuge as the setting separation factor of the ultracentrifuge; before weighing 5-10 g of the soybean phospholipid sample into the centrifuge tube, the method further comprises: mapping the weighed soybean phospholipid sample to obtain its surface morphology; constructing a three-dimensional model of the soybean phospholipid sample according to the surface morphology and the mapping parameters; performing mesh scanning on the three-dimensional model, and determining whether the soybean phospholipid sample is hollow according to the scanning result, if yes, it is determined that the soybean phospholipid sample does not meet the test requirements, otherwise, it is preliminarily determined that the soybean phospholipid sample meets the test requirements; immersing the soybean phospholipid sample in water for a target time, analyzing the composition of the soaked water, and obtaining an analysis result; determining sensitive parameters in the soybean phospholipid sample according to the analysis result; testing the influence value of each sensitive parameter on the n-hexane dissolution rate; constructing a dissolution degradation trajectory model of n-hexane under the sensitive parameters according to the influence value; calculating an error factor of the final HI value through the dissolution degradation trajectory model; evaluating whether the soybean phospholipid sample is qualified according to the error factor, if yes, the soybean phospholipid sample is used as a test sample, otherwise, the soybean phospholipid sample is repeatedly selected and tested until it passes the test.

2. The method of analyzing the HI value of a liquid soybean phospholipid product according to claim 1, characterized by, The centrifuge tube rotor cover of the ultracentrifuge adopts a double locking structure.

3. The method of analyzing the HI value of a liquid soybean phospholipid product according to claim 1, characterized by, The centrifugal force of the ultracentrifuge is determined by the following method: detecting the density of each of the particles and the solution and the viscosity of the solution in the mixture of the soybean phospholipid sample and n-hexane; According to the density of each of the particles and the solution in the mixture of the soybean phospholipid sample and the n-hexane and the viscosity of the solution, the settling velocity of the soybean phospholipid sample in the n-hexane is calculated: ； wherein, is the sedimentation velocity of the sample of soybean phospholipids in the n-hexane, is the particle density in the mixture of the sample of soybean phospholipids and n-hexane, is the solution density in the mixture of the sample of soybean phospholipids and n-hexane, d is the maximum particle diameter in the mixture of the sample of soybean phospholipids and n-hexane, is the solution viscosity in the mixture of the sample of soybean phospholipids and n-hexane; According to the settling velocity of the soybean phospholipid sample in the n-hexane, a corresponding target centrifugal force is selected as the setting centrifugal force of the ultracentrifuge.

4. The method of analyzing the HI value of a liquid soybean phospholipid product according to claim 1, characterized by, The repeated centrifugal precipitation operation is performed 2-3 times on the precipitate to obtain a sample residue, including: According to the second proportion, the n-hexane is added to the centrifuge tube to perform the repeated centrifugal precipitation operation 2-3 times to obtain the sample residue.

5. The method of analyzing the HI value of a liquid soybean phospholipid product according to claim 1, characterized by, The vacuum drying is performed on the sample residue, and after the drying is completed, the hexane-insoluble content (HI) value in the sample residue is calculated, including: The vacuum drying temperature and the drying duration are set; According to the vacuum drying temperature and the drying duration, the vacuum drying is performed on the sample residue until the sample residue meets a determination condition, and the determination condition is that the sample residue maintains a constant weight during the vacuum drying; The sample mass of the soybean phospholipid sample, the centrifuge tube mass, and the total mass of the centrifuge tube and the vacuum-dried sample residue are obtained; According to the sample mass of the soybean phospholipid sample, the centrifuge tube mass, and the total mass of the centrifuge tube and the vacuum-dried sample residue, the hexane-insoluble content (HI) ratio of the soybean phospholipid sample is calculated: ； wherein X represents the hexane insolubles content (HI) of the soybean phospholipid sample divided by the total sample mass, represents the total mass of the sample residue after centrifugation and vacuum drying, represents the mass of the centrifuge tube, represents the sample mass of the soybean phospholipid sample.

6. A system for analyzing the HI value of a liquid soybean phospholipid product, characterized by, The system comprises: A first obtaining module is configured to obtain a liquid soybean phospholipid sample dissolved by ultrasonic waves; A precipitation module is configured to perform centrifugal precipitation on the liquid soybean phospholipid sample by using an ultracentrifuge; A second obtaining module is configured to perform repeated centrifugal precipitation operation 2-3 times on the precipitate to obtain a sample residue; A calculation module is configured to perform vacuum drying on the sample residue, and after the drying is completed, calculate the hexane-insoluble content (HI) value in the sample residue; The liquid soybean phospholipid sample dissolved by ultrasonic waves comprises: 5-10 g of soybean phospholipid sample is weighed into a centrifuge tube; According to a first proportion, n-hexane is added to the centrifuge tube for dissolution; Real-time dissolution efficiency during the dissolution process is detected; It is determined whether the real-time dissolution efficiency is greater than or equal to a preset threshold value, if yes, no subsequent operation is needed, otherwise, auxiliary dissolution is performed by using ultrasonic waves to obtain a liquid soybean phospholipid sample dissolved by ultrasonic waves; The liquid soybean phospholipid sample is centrifuged by using the ultracentrifuge to obtain supernatant and precipitate, including: The separation factor, centrifugal force, centrifugal time, and centrifugal temperature of the ultracentrifuge are set; After the setting is completed, the centrifuge tube is sealed by using the centrifuge tube rotor cover of the ultracentrifuge; The ultracentrifuge is started to centrifugally precipitate the mixture of the soybean phospholipid sample and the n-hexane in the centrifuge tube to obtain the supernatant and the precipitate; The separation factor of the ultracentrifuge is determined by the following method: The factory parameters of the ultracentrifuge are obtained; According to the factory parameters, the drum radius and the running speed interval of the drum of the ultracentrifuge are determined; According to the drum radius and the running speed interval of the drum of the ultracentrifuge, the separation factor setting interval of the ultracentrifuge is calculated: ； wherein represents the minimum separation factor or the maximum separation factor of the ultracentrifuge, represents the circle constant with a value of 3.14, and r represents the radius of the bowl of the ultracentrifuge, represents the minimum or maximum rotational speed in the operating rotational speed interval of the bowl of the ultracentrifuge, and g represents the acceleration due to gravity; In the separation factor setting interval of the ultracentrifuge, a target separation factor greater than or equal to 15000G is selected as the setting separation factor of the ultracentrifuge; The system is also used for: plotting the surface morphology of the soybean phospholipid sample; constructing a three-dimensional model of the soybean phospholipid sample according to the surface morphology and the plotting parameters; performing a mesh scan on the three-dimensional model to determine whether the soybean phospholipid sample is hollow inside, and if so, confirming that it does not meet the testing requirements, otherwise, preliminarily confirming that it meets the testing requirements; immersing the soybean phospholipid sample in water for a target duration, and performing component analysis on the soaked water to obtain analysis results; determining sensitive parameters in the soybean phospholipid sample according to the analysis results; testing the influence value of each sensitive parameter on the n-hexane solubility; constructing a n-hexane solubility degradation trajectory model under the sensitive parameters according to the influence value; calculating an error factor of the final HI value through the solubility degradation trajectory model; evaluating whether the soybean phospholipid sample is qualified according to the error factor, and if so, using it as a test sample, otherwise, reselecting a soybean phospholipid sample to repeat the above test until it passes the test.

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