CN115469041B - One-measurement-multiple-evaluation content determination method for nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation - Google Patents
One-measurement-multiple-evaluation content determination method for nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation Download PDFInfo
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Abstract
The invention discloses a one-measurement-multi-evaluation content determination method for a nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation, which adopts a UPLC-MS/MS method to simultaneously determine the content of 16 chemical components in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation. The method can rapidly and effectively measure the contents of 16 components in the nine-ingredient blood-replenishing oral liquid, has high sensitivity, good specificity and reproducibility, and accurate and reliable detection results, and provides an effective method for improving the quality control technical level and the sound quality control system of the nine-ingredient blood-replenishing oral liquid, thereby ensuring the quality uniformity, stability, clinical curative effect and safety of the nine-ingredient blood-replenishing oral liquid.
Description
Technical Field
The invention belongs to the technical field of traditional Chinese medicine quality control, and relates to a one-measurement-multiple-evaluation content determination method for a nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation.
Background
The nine-ingredient blood-replenishing oral liquid is composed of 9 medicinal materials such as ginseng, astragalus root, gynostemma pentaphylla and the like, has the effects of replenishing qi and blood, strengthening spleen and replenishing stomach, and has good effects of replenishing qi and blood and promoting sleep, and is used for treating insomnia and amnesia caused by deficiency of both qi and blood, palpitation and secondary, dizziness, listlessness, short qi and spontaneous perspiration, anorexia and the like. The invention discloses a preparation method and application of a traditional Chinese medicine preparation, and discloses publication number CN1883593A, and the invention name of the nine-ingredient blood-replenishing oral liquid.
The basic research of the nine-ingredient blood-replenishing oral liquid is relatively less, and the existing quality standard
[ YBZ00362007-2015Z ] and literature receiving or reporting thin-layer identification of medicinal materials such as angelica sinensis, liquorice, dried orange peel, ginseng, gynostemma pentaphylla, astragalus membranaceus, schisandra chinensis and the like, and content measurement of ferulic acid in angelica sinensis, schisandra chinensis methyl and astragaloside in astragalus membranaceus, wherein the quality control method of the components is relatively single, and lacks systematicness and comprehensiveness. Therefore, the research and development of the material basis of the nine-ingredient blood-replenishing oral liquid are in progress, and a content measuring method for simultaneously measuring various active ingredients in the nine-ingredient blood-replenishing oral liquid is imperative as a quality control means. The invention researches and establishes and verifies a method for simultaneously measuring the contents of various components in the nine-ingredient blood-replenishing oral liquid based on an ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS/MS) technology, and the method is quick, accurate, high in sensitivity, strong in specificity and good in reproducibility, provides a reliable technology for establishing a perfect quality control technology and a quality control system of the whole production process, improves the quality control level of the nine-ingredient blood-replenishing oral liquid, and ensures the quality and clinical curative effect of the product.
Disclosure of Invention
The invention aims to provide a one-measurement-multiple-evaluation content measuring method for a nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation, which is a measuring method for simultaneously measuring the contents of various ingredients in a nine-ingredient blood-replenishing oral liquid of a traditional Chinese medicine compound preparation for replenishing qi and replenishing blood and promoting sleep based on an ultra-high performance liquid chromatography-mass spectrometry (UPLC-MS) technology, and establishes a content measuring method capable of simultaneously measuring 16 main ingredients in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation so as to improve the quality control level of the nine-ingredient blood-replenishing oral liquid.
In order to achieve the purpose of the invention, the invention adopts the following technical proposal and steps:
a method for measuring the content of one or more evaluation components of a nine-ingredient blood-replenishing oral liquid Chinese medicinal preparation adopts a UPLC-MS/MS method, and simultaneously measures the content of 16 chemical components in the nine-ingredient blood-replenishing oral liquid Chinese medicinal preparation;
(1) Establishing standard curves of 16 chemical components;
(2) Obtaining a multi-reaction ion chromatogram of 16 chemical components in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation, precisely sucking 1ml of the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation, placing in a 20ml volumetric flask, adding methanol, carrying out ultrasonic dissolution, fixing the volume to a scale, shaking uniformly, filtering by a filter membrane, and taking a subsequent filtrate as a sample solution;
under the same chromatographic conditions and mass spectrum conditions as in the step (1), the sample solution is injected into a liquid chromatograph-mass spectrometer to obtain a multi-reaction ion chromatogram of each chemical component in the compound preparation;
(3) Determination of 16 chemical component contents in nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation
And determining the content of each chemical component in the compound preparation according to the peak area of the multi-reaction ion chromatogram of each chemical component in the nine-component blood-replenishing oral liquid traditional Chinese medicine preparation and the standard curve of the corresponding chemical component.
The 16 chemical components comprise: ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rd, astragaloside IV, calycosin, hesperidin, naringin, hesperetin, nobiletin, schizandrin A, schizandrin B, schizandrin A, Z-ligustilide, glycyrrhizin, and ammonium glycyrrhizinate.
The step (1) of establishing a standard curve of 16 chemical components is as follows: respectively precisely weighing reference substances such as ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rd, astragaloside IV, calycosin, hesperidin, naringin, hesperetin, nobiletin, schizandrin A, schizandrin B, schizandrin A, ligustilide, glycyrrhizin and ammonium glycyrrhizinate, dissolving with 95% methanol to obtain reference substance stock solutions with certain concentration; precisely sucking 16 reference substance stock solutions respectively, and diluting with 95% methanol to obtain a series of reference substance mixed solutions of 16 chemical components with different concentrations; under the set chromatographic conditions and mass spectrum conditions, respectively injecting the mixed solutions of the reference substances with various concentrations into a liquid chromatograph-mass spectrometer to obtain multi-reaction ion chromatograms of the reference substances with different concentrations; and (3) taking the chromatographic peak area of each reference substance as an ordinate and the concentration of each reference substance as an abscissa, and obtaining the standard curve of each chemical component through linear regression operation.
The chromatographic conditions set are: the chromatographic column adopts a stationary phase of octadecylsilane chemically bonded silica gel; mobile phase: phase A is 0.1% formic acid or water, phase B is acetonitrile; gradient elution; column temperature: 30 ℃; flow rate: 0.3mL/min; sample injection amount: 1 μl;
the elution procedure was: 0-5min,2% B;5-30min,2% -80% B;30-35min,80% -95% B.
The set mass spectrum conditions include:
ionization mode: electrospray ionization; a multi-reaction ion monitoring mode, a full scanning mode; ion spray voltage: -4500V or 5500V; ion source pressure: 15psi; air curtain air pressure: 20psi; drying gas and atomizing gas: nitrogen gas.
Mass spectrometry conditions and ion modes are as follows:
in one embodiment of the present invention, the concentration of each control at S/n=3 and S/n=10 is used as the lowest detection limit and the lowest quantification limit, respectively.
The invention adopts UPLC-MS/MS method to measure the content of 16 chemical components in the nine-ingredient blood-replenishing oral liquid, has the characteristics of high sensitivity, strong reliability, high efficiency and rapidness, and can more effectively control the quality of the nine-ingredient blood-replenishing oral liquid by measuring the content of 16 chemical components in the nine-ingredient blood-replenishing oral liquid, thereby ensuring the clinical curative effect of the nine-ingredient blood-replenishing oral liquid.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below.
FIG. 1 is a multi-reaction ion chromatogram of ligustilide in a control at a certain concentration;
FIG. 2 is a multi-reactive ion chromatogram of calycosin at a concentration in a control;
FIG. 3 is a multi-reactive ion chromatogram of hesperetin at a certain concentration in a control;
FIG. 4 is a multi-reaction ion chromatogram of nobiletin in a control at a certain concentration;
FIG. 5 is a multi-reaction ion chromatogram of schisandrin A in a control at a certain concentration;
FIG. 6 is a multi-reaction ion chromatogram of schisandrin A in a control at a certain concentration;
FIG. 7 is a multi-reaction ion chromatogram of schisandrin B in a control at a certain concentration;
FIG. 8 is a multi-reaction ion chromatogram of astragaloside IV in a control at a certain concentration;
FIG. 9 is a multi-reaction ion chromatogram of glycyrrhizin at a given concentration in the control;
FIG. 10 is a multi-reactive ion chromatogram of naringin at a concentration in a control;
FIG. 11 is a multi-reactive ion chromatogram of hesperidin at a certain concentration in a control;
FIG. 12 is a multi-reactive ion chromatogram of ammonium glycyrrhetate in a control at a concentration;
FIG. 13 is a multi-reaction ion chromatogram of ginsenoside Rg1 in a control at a certain concentration;
FIG. 14 is a multi-reaction ion chromatogram of ginsenoside Re at a certain concentration in the reference;
FIG. 15 is a multi-reaction ion chromatogram of ginsenoside Rd at a certain concentration in the control;
FIG. 16 is a multi-reaction ion chromatogram of ginsenoside Rb1 in a control at a certain concentration;
FIG. 17 is a multi-reaction ion chromatogram of ligustilide in a test sample of the nine-ingredient blood-replenishing oral liquid at a certain concentration;
FIG. 18 is a multi-reaction ion chromatogram of calycosin at a given concentration in a test sample of a nine-ingredient blood-replenishing oral liquid;
FIG. 19 is a multi-reactive ion chromatogram of hesperetin at a certain concentration in a test sample of the nine-ingredient blood replenishing oral liquid;
FIG. 20 is a multi-reaction ion chromatogram of nobiletin in a nine-ingredient blood replenishing oral liquid test sample at a certain concentration;
FIG. 21 is a multi-reaction ion chromatogram of schisandrin A in a certain concentration in a test sample of the nine-ingredient blood replenishing oral liquid;
FIG. 22 is a multi-reaction ion chromatogram of schisandrin A in a test sample of the nine-ingredient blood-replenishing oral liquid;
FIG. 23 is a multi-reaction ion chromatogram of schisandrin B in a certain concentration in a nine-ingredient blood replenishing oral liquid test sample;
FIG. 24 is a multi-reaction ion chromatogram of astragaloside IV in a nine-ingredient blood-replenishing oral liquid test sample at a certain concentration;
FIG. 25 is a multi-reactive ion chromatogram of glycyrrhizin in a test sample of the nine-ingredient blood-replenishing oral liquid at a certain concentration;
FIG. 26 is a multi-reactive ion chromatogram of naringin at a concentration in a test sample of a nine-ingredient blood-replenishing oral liquid;
FIG. 27 is a multi-reactive ion chromatogram of hesperidin at a certain concentration in a test sample of the Jiuwei blood replenishing oral liquid;
FIG. 28 is a multi-reaction ion chromatogram of ammonium glycyrrhizate in a nine-ingredient blood-replenishing oral liquid test sample at a certain concentration;
FIG. 29 is a multi-reaction ion chromatogram of ginsenoside Rg1 in a nine-ingredient blood replenishing oral liquid test sample at a certain concentration;
FIG. 30 is a multi-reaction ion chromatogram of ginsenoside Re in a nine-ingredient blood replenishing oral liquid test sample at a certain concentration;
FIG. 31 is a multi-reaction ion chromatogram of ginsenoside Rd at a certain concentration in a test sample of the nine-ingredient blood-replenishing oral liquid;
fig. 32 is a multi-reaction ion chromatogram of ginsenoside Rb1 in a test sample of the Jiuwei blood replenishing oral liquid at a certain concentration.
Detailed Description
The advantages and the spirit of the present invention will be better understood by reference to the following examples, which are not intended to limit the invention.
The following are relevant test instruments, standards, reagents and samples used in the examples:
experimental instrument:
an ultra-high performance rapid liquid chromatography system (ExionLC AD) comprising an on-line vacuum degasser, a binary pump, an automatic sampler and a column incubator (Shimadzu);
sciex triple quaternary tandem mass spectrometry detector (SCIEX QTRAP Triple Quad 5500+), containing electrospray ion source (ESI source), analysis software (Sciex, USA);
chromatographic column: waters ACQUITY UPLC HSS T3 (2.1 mm. Times.100 mm,1.8 μm) (Waters, america).
Milli-Q deionized water System (Millipore, U.S.A.); KQ-500DB type numerical control ultrasonic cleaner.
Control: ginsenoside Rg1 (lot number: 110703-202034), ginsenoside Re (lot number: 110754-202129), ginsenoside Rb1 (lot number: 110704-202028), astragaloside IV (lot number: 110781-202118), schizandrin A (lot number: 110857-201815), ligustilide (lot number: 111737-201910) are all purchased from Chinese food and drug assay institute; ginsenoside Rd (lot number: 5826), hesperidin (lot number: 5836), naringin (lot number: 10668), glycyrrhizin (lot number: 9654), ammonium glycyrrhizinate (lot number: 10845), hesperetin (lot number: 10027), nobiletin (lot number: 6082), schizandrin (lot number: 8366), calycosin (lot number: 10659), and schizandrin A (lot number: 7954) were all purchased from Shanghai Shimadder standard technical services Co.
HPLC grade acetonitrile, HPLC grade methanol, HPLC grade formic acid (Fisher, usa); deionized water;
nine-ingredient blood replenishing oral liquid sample: 6 different batches of nine-ingredient blood-replenishing oral liquid are produced by Yingkang pharmaceutical industry Co., ltd.
Example 1 the establishment of a method for simultaneously measuring the contents of various components in a nine-ingredient blood-replenishing oral liquid based on UPLC-MS technology.
1. Preparation of test solutions
Precisely sucking 1ml of the product, placing in a 20ml volumetric flask, adding appropriate amount of methanol, ultrasonic dissolving, fixing volume to scale, shaking, filtering with a filter membrane, and collecting the filtrate as sample solution.
The invention discloses a method for preparing a nine-ingredient blood replenishing oral liquid, which comprises the steps of qualitatively researching main components in a nine-ingredient blood replenishing oral liquid sample solution by adopting ACQUITY I-CLASS Plus ultra-high performance liquid chromatography-XeFo G2-XS four-pole time-of-flight mass spectrum (Waters company in the United states), and totally separating 136 compounds mainly comprising saponins, lignans, flavonoids, phthalides, terpenes, organic acids and other compounds.
2. Carrying out UPLC-MS detection analysis on the nine blood replenishing oral liquid sample solution:
chromatographic conditions: the ExionLC AD ultra-high performance rapid liquid chromatography system comprises a chromatographic column which is HSS T3 (2.1 mm ×100mm,1.8 μm), a column temperature of 30 ℃, a flow rate of 0.3mL/min, a sample injection volume of 1 μL, a mobile phase A which is 0.1% formic acid (positive ion mode) or water (negative ion mode), a mobile phase B which is acetonitrile, and gradient elution conditions: 0-5min,2% B;5-30min,2% -80% B;30-35min,80% -95%.
Mass spectrometry conditions: sciex triple quaternary tandem mass spectrometry detector, analysis software (Sciex, USA); ionization mode: electrospray ionization; a multi-reaction ion monitoring mode, a full scanning mode; ion spray voltage: -4500V or 5500V; ion source pressure: 15psi; air curtain air pressure: 20psi; drying gas and atomizing gas: nitrogen gas. The cleavage process of a compound from a parent ion to a specific daughter ion is monitored quantitatively using a Multiplex Reaction Monitoring (MRM) mode.
The optimized MRM conditions are shown in Table 1.
Table 1: MRM parameters of 16 compounds in nine-ingredient blood-replenishing oral liquid
TABLE 1
3. Methodology investigation
(1) Standard curve, quantitative limit and detection limit
And respectively precisely sucking the mixed stock solution of the reference substances, diluting the mixed stock solution into a series of mixed reference substance solutions (n=6) with concentration gradients by using 95% methanol, and carrying out 1 mu L analysis on each concentration of the reference substances to obtain multi-reaction ion chromatograms of the reference substances at different concentrations, and carrying out linear regression on the concentrations by using chromatographic peak areas of the reference substances to obtain standard curves of the components.
The mixed control solutions were diluted stepwise, and the concentrations of the controls at S/n=3 and S/n=10 were used as the detection Limit (LOD) and the quantification Limit (LOQ), respectively. The results are shown in Table 2, and the experimental results show that the linear correlation coefficient of each compound is good, and the quantitative limit and the detection limit meet the detection requirements.
TABLE 2 Standard Curve, linear Range, detection Limit and quantitative Limit of 16 Compounds in nine-ingredient blood replenishing oral liquid
(2) Precision, repeatability, stability
Precisely transferring 1ml of the nine-ingredient blood replenishing oral liquid, placing in a 20ml volumetric flask, adding a proper amount of methanol, performing ultrasonic dissolution, fixing the volume to a scale, shaking uniformly, filtering with a filter membrane, and taking the subsequent filtrate as a sample solution. Repeating sample injection for 6 times according to the chromatographic conditions, measuring the concentration of each component, and calculating the RSD value of the component to examine the precision of the instrument.
Precisely transferring 1ml of the nine-ingredient blood replenishing oral liquid, placing in a 20ml volumetric flask, adding a proper amount of methanol, performing ultrasonic dissolution, fixing the volume to a scale, shaking uniformly, filtering with a filter membrane, and taking the subsequent filtrate as a sample solution. 6 parts of the sample are prepared in parallel, the concentration of each component is measured by sampling according to the chromatographic conditions, and the RSD value of each component is calculated to investigate the repeatability of the method.
Precisely transferring 1ml of the nine-ingredient blood replenishing oral liquid, placing in a 20ml volumetric flask, adding a proper amount of methanol, performing ultrasonic dissolution, fixing the volume to a scale, shaking uniformly, filtering with a filter membrane, and taking the subsequent filtrate as a sample solution. After the sample is placed at room temperature for 0,3,6, 12 and 24 hours, samples are taken according to the chromatographic conditions, the concentration of each component is measured, and the RSD value of the sample is calculated, so that the stability of the 16 components in the sample solution at room temperature is examined.
The results of the precision, repeatability and stability examination are shown in table 3, and the experimental results show that the results all meet the detection requirements.
(3) Accuracy of
The sample is recovered and measured. Precisely removing 0.5ml of nine-ingredient blood replenishing oral liquid, placing in a 20ml capacity bottle, respectively adding a certain amount of mixed reference substance solution containing 16 ingredients, fixing volume to scale with 95% methanol, shaking, filtering with a filter membrane, and collecting the subsequent filtrate as sample solution. 6 parts of the sample are prepared in parallel, sample injection is carried out according to the chromatographic conditions, the concentration of each component is measured, and the sample injection recovery rate and the RSD value are calculated to investigate the accuracy of the method.
The accuracy inspection results are shown in table 3, and the experimental results show that the method meets the detection requirements.
Table 3 precision, repeatability, stability and accuracy of 16 compounds in nine-ingredient blood replenishing oral liquid
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EXAMPLE 2 Simultaneous determination of 16 component contents in nine-ingredient blood-replenishing oral liquid sample
According to the method established in example 1, 6 batches of nine-ingredient blood-replenishing oral liquid were subjected to content measurement. The preparation method of the test solution of the nine-ingredient blood replenishing oral liquid in 6 batches comprises the following steps: precisely transferring 1ml of the nine-ingredient blood replenishing oral liquid, placing in a 20ml volumetric flask, adding a proper amount of methanol, performing ultrasonic dissolution, fixing the volume to a scale, shaking uniformly, filtering with a filter membrane, and taking the subsequent filtrate as a sample solution. 1. Mu.L of each sample was introduced under the above chromatographic conditions, the peak area of the measured component was recorded, the content (CA,. Mu.g/mL) was calculated by substituting the peak area into a standard curve, and the content of the compound in the nine-ingredient blood-replenishing oral liquid was calculated from CA X20, and the results are shown in Table 4.
Table 4 6 the contents of 16 Compounds (μg/mL) in nine-ingredient blood-replenishing oral liquid samples
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In conclusion, the method for simultaneously measuring the contents of various components in the nine-ingredient blood-replenishing oral liquid based on the UPLC-MS/MS technology has good precision, repeatability and accuracy; the technical scheme of the invention has feasibility and advancement. The determination method of the invention can further improve the quality control level of the nine-ingredient blood-replenishing oral liquid.
Claims (2)
1. A method for measuring the one-measurement-multiple-evaluation content of a nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation is characterized in that a UPLC-MS/MS method is adopted, and the content of 16 chemical components in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation is measured simultaneously;
(1) Establishing standard curves of 16 chemical components;
(2) Obtaining a multi-reaction ion chromatogram of 16 chemical components in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation, precisely sucking 1ml of the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation, placing in a 20ml volumetric flask, adding methanol, carrying out ultrasonic dissolution, fixing the volume to a scale, shaking uniformly, filtering by a filter membrane, and taking a subsequent filtrate as a sample solution;
under the same chromatographic conditions and mass spectrum conditions as those in the step (1), the sample solution is injected into a liquid chromatograph-mass spectrometer to obtain a multi-reaction ion chromatogram of each chemical component in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation;
(3) Determining the content of 16 chemical components in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation;
determining the content of each chemical component in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation according to the peak area of the multi-reaction ion chromatogram of each chemical component in the nine-ingredient blood-replenishing oral liquid traditional Chinese medicine preparation and the standard curve of the corresponding chemical component;
the 16 chemical components comprise: ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rd, astragaloside IV, calycosin, hesperidin, naringin, hesperetin, nobiletin, schizandrin A, schizandrin B, schizandrin A, Z-ligustilide, glycyrrhizin, ammonium glycyrrhizinate;
the chromatographic conditions set are: the chromatographic column adopts a stationary phase of octadecylsilane chemically bonded silica gel; mobile phase: phase A is 0.1% formic acid or water, phase B is acetonitrile; gradient elution; column temperature: 30 ℃; flow rate: 0.3mL/min; sample injection amount: 1 μl;
the elution procedure was: 0-5min,2% B;5-30min,2% -80% B;30-35min,80% -95% B;
the set mass spectrum conditions include:
ionization mode: electrospray ionization; a multi-reaction ion monitoring mode, a full scanning mode; ion spray voltage: -4500V or 5500V; ion source pressure: 15psi; air curtain air pressure: 20psi; drying gas and atomizing gas: nitrogen gas;
mass spectrometry conditions and ion modes are as follows:
。
2. the method of claim 1, wherein the step of establishing a standard curve of 16 chemical components in step (1) is: precisely weighing reference substances of ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, ginsenoside Rd, astragaloside IV, calycosin, hesperidin, naringin, hesperetin, nobiletin, schizandrin A, schizandrin B, schizandrin A, ligustilide, glycyrrhizin and ammonium glycyrrhizinate respectively, dissolving with 95% methanol to obtain reference substance stock solutions with certain concentration; precisely sucking 16 reference substance stock solutions respectively, and diluting with 95% methanol to obtain a series of reference substance mixed solutions of 16 chemical components with different concentrations; under the set chromatographic conditions and mass spectrum conditions, respectively injecting the reference substance mixed solution with each concentration into a liquid chromatography-mass spectrometer to obtain multi-reaction ion chromatograms of the reference substances under different concentrations; and (3) taking the chromatographic peak area of each reference substance as an ordinate and the concentration of each reference substance as an abscissa, and obtaining the standard curve of each chemical component through linear regression operation.
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| 超高效液相串联质谱检测茶叶及茶饮料中咖啡因含量;秦园;王惠芳;吴建兵;钱志荣;吴梅;陈祝军;;食品工业科技(第10期);第286-289、301页 * |
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