CN100371706C - Method for investigating Monacolin kind compound content in functional Monacolin - Google Patents
Method for investigating Monacolin kind compound content in functional Monacolin Download PDFInfo
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- CN100371706C CN100371706C CNB200610086801XA CN200610086801A CN100371706C CN 100371706 C CN100371706 C CN 100371706C CN B200610086801X A CNB200610086801X A CN B200610086801XA CN 200610086801 A CN200610086801 A CN 200610086801A CN 100371706 C CN100371706 C CN 100371706C
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Abstract
The present invention relates to a method for detecting the content of functional red rice monacolin type compounds, which comprises the following steps: 1) pretreatment of samples; 2) acid type monacolin K standard sample preparation; 3) chromatogram sampling analysis; 4) graph spectrum analysis and result calculation. In the method, the functional red rice monacolin type compounds are well separated by a liquid phase chromatograph with high efficiency, ultraviolet absorption spectrums of all the monacolin type compounds are detected by a diode array detector, the performance of the functional red rice monacolin type compounds can be determined by using an external standard method according to the retention time and an ultraviolet absorption spectrum graph, and the content of the functional red rice monacolin type compounds is determined by peak areas. The method can detect the total content of the monacolin type compounds in the samples by detecting the joint characteristic of the ultraviolet absorption spectrums of the monacolin type compounds in the samples under the condition of monacolin compound standard sample shortage. The method has the advantages of favorable accuracy, precision and linear relation, and can obtain a good result on detecting functional red rice samples.
Description
Technical Field
The invention relates to a method for detecting functional components of health-care food.
Background
Red yeast rice is widely used in food industry as natural pigment and food additive. In 1979, monacolin K is reported to be separated from Monascus fermentation liquor and has the effect of reducing plasma cholesterol, and has the effect of inhibiting the synthesis of cholesterol in human bodies. Later researches prove that Monacolin can generate substances which have inhibitory activity on 3-hydroxy-3-methylglutaryl coenzyme A reductase (HMG-CoA reductase) of animals and human bodies, namely Monacolin compounds, in the later growth period of the Monacolin. They are a family of structural analogues that can be classified as: monacolin J, K, L, X, M, dihydromevinolin, dihydromonoacolin L and the like. Wherein the content of Monacolin K is the maximum.
Because the Monacolin substances have obvious effect of inhibiting the synthesis of cholesterol, small toxic and side effect and good tolerance, the Monacolin substances can be quickly applied to clinic from discovery. In recent years, the Monacolin compound is popular among consumers as an effective component of health food for application to some health food with the function of reducing blood fat. In order to ensure the product quality, the method is very important for detecting Monacolin substances in raw materials and products.
Since 2000, methods for measuring the content of Monacolin K (also called Lovastatin) in red yeast rice by using an ultraviolet spectrophotometer and a reversed phase high performance liquid chromatography-ultraviolet detector have been reported in China food additive and journal of food science successively by laboratories. The ultraviolet detector can only obtain the chromatogram outflow curve chart of each component under a single wavelength, but cannot obtain the absorption spectrogram of each component flowing out along with the chromatogram components; and because many standard samples of Monacolin compounds are not commercially available at present, the characterization of each separated component is difficult. Therefore, only Monacolin K with the most content in Monacolin compounds is actually measured for the quantitative determination of the blood fat reducing functional factors in the red yeast rice, and other Monacolin compounds in the red yeast rice are ignored. This is clearly deficient for the accurate assessment of functional factors inhibiting cholesterol synthesis in red yeast rice.
Disclosure of Invention
In order to solve the problems, the invention provides a method for detecting the content of Monacolin compounds in functional red yeast rice. The invention is realized by the following steps:
a method for detecting the content of Monacolin compounds in functional red yeast rice comprises the following steps:
1) Sample pretreatment;
2) Preparing an acid Monacolin K standard sample;
3) Carrying out chromatographic sample injection analysis;
4) And (4) carrying out spectrum analysis and result calculation.
The method for detecting the content of the Monacolin compounds in the functional red yeast rice comprises the following specific steps:
1) The sample pretreatment step comprises: crushing a red yeast sample (more than or equal to 80 meshes) and fully and uniformly mixing; accurately weighing 400.0-600.0mg of sample in a 50ml volumetric flask, adding 30ml of 75% ethanol (V/V), shaking uniformly, and performing ultrasonic treatment at room temperature for 20min (the working frequency is 40 KHz). Adding 75% ethanol to approximate scale, performing ultrasonic treatment for 10min, cooling to room temperature, and diluting to 50ml with 75% ethanol; centrifuging at 3500 rpm/min for 10min; taking supernatant fluid, passing through a 0.45 mu m pore diameter microporous filter membrane, and waiting for sample injection of filtrate;
2) The preparation method of the acid Monacolin K standard sample comprises the following steps: weighing 4mg of Monacolin K (lactone) standard, fixing the volume to 100ml by using 0.2M sodium hydroxide solution, carrying out ultrasonic transformation for 1 hour at 50 ℃, cooling to room temperature, and standing in the dark for 3 hours for use; calculating the conversion rate according to the chromatographic peak areas of the converted acid type Monacolin K and the residual lactone Monacolin K; accurately determining the quality and quantity of the acid Monacolin K in the sample by using the prepared acid Monacolin K;
3) The chromatographic sample injection analysis step comprises: taking the filtrate filtered by the microporous membrane into a liquid chromatograph, wherein the chromatographic conditions of the chromatograph are as follows: a chromatographic column: c 18 Column, 4.6X 250mm,5 μm; column temperature: room temperature; IIA polar tube array detector: scanning at 200-350nm, and processing data by a chromatogram at 238 nm; mobile phase: methanol: water: phosphoric acid = 385: 115: 0.14 (V: V); flow rate: 1.0ml/min; sample introduction amount: 20 mu l of the mixture;
4) The map analysis and result calculation steps comprise: finding component peaks which have the same ultraviolet absorption spectrum with standard Monacolin K on a chromatogram outflow curve chart, namely Monacolin compounds, adding the peak areas of the components, comparing the peak areas with the standard Monacolin K chromatogram peak area, and calculating the total amount of the Monacolin compounds in the sample;
the resulting calculation formula:
in the formula: total amount of Monacolin compounds in X-form, mg/g
h 1 Sum of the areas of the chromatographic peaks of the separated fractions having a characteristic absorption spectrum of the Monacolin type of compounds
c-Standard Monacolin K (lactone type or acid type) solution concentration, mg/ml
50-volume fixed volume of sample, ml
h 2 Peak area of MonacolinK (lactone type or acid type)
m-sample weighing, g.
The functional red yeast fermentation product contains various Monacolin compounds, and is mainly in lactone type and acid type Monacolin K. During the dehydration drying treatment, the acid form of Monacolin K is gradually converted into the lactone form. Because of their physiological activity, it is more meaningful to measure the total amount of Monacolin compounds.
The diode array detector can give the real-time ultraviolet absorption spectrum of all separated component chromatogram outflow, so that the condition that the Monacolin compounds with the same ultraviolet absorption spectrum as the Monacolin K are separated can be clearly seen on a chromatogram outflow curve chart. If standard substances exist, the qualitative determination and the quantitative determination of the standard substances are very convenient. For example, no standard substance is currently on the market due to the instability of the acid form of Monacolin K. The standard lactone type Monacolin K can be conveniently converted into acid form by utilizing the conditions provided by the method. The converted standard sample is used for sample injection, so that the acid Monacolin K in the sample can be accurately determined qualitatively and quantitatively.
The total amount of Monacolin compounds in the sample can be obtained by adding the peak areas of the Monacolin compounds having the same UV absorption spectrum as that of Monacolin K and quantifying them with a standard lactone type Monacolin K. Although the response of different Monacolin compounds to the detector may vary, and the results obtained may have some errors, this method is effective in the absence of the Monacolin-based compound standard. And because various Monacolin compounds in the sample are mainly in lactone type and acid type Monacolin K, and lactone type Monacolin K is sold in the market, the method also solves the preparation problem of acid type Monacolin K standard samples, and the content of other Monacolin compounds is very small, so the method has higher accuracy in determining the total amount of the Monacolin compounds in the functional red yeast rice sample.
If the content of effective components in the sample is too low, the supernatant after extraction and centrifugation can be properly concentrated by a reduced pressure concentration method, but the result needs to be calculated according to the accurate volume after concentration.
The invention will be further described with reference to the accompanying drawings.
Drawings
FIG. 1 shows the standard chromatograms of Monacolin K (lactone form) and Monacolin K acid (ring-opened acid form)
FIG. 2 is chromatogram of a sample of red yeast rice
FIG. 3 is a Monacolin k standard curve
Detailed Description
Detection of Monacolin compound content in functional red yeast rice
1. Material
1.1 reagents
1.1 chromatographic purification of methanol
1.2 Anhydrous ethanol analytical purity
1.3 analytical purification of phosphoric acid
1.4 analytical purification of sodium hydroxide
1.5 The Monacolin K standard solution is accurately weighed to be 40.0mg of Monacolin K (lactone type) standard substance, and the volume is 100ml by mobile phase. The concentration of this solution was 400. Mu.g/ml.
1.6 1ml of Monacolin K standard stock solution is accurately measured from the Monacolin K standard working solution, and 10ml of mobile phase constant volume is adopted. The concentration of this solution was 40. Mu.g/ml.
1.2 instrumentation
1.2.1 high performance liquid chromatograph (Waters 600E)
1.2.2 diode Array Detector (Photodiode Array Detector, waters 2996)
1.2.3 Low-speed centrifuge (Shanghai surgical instruments factory, 80-2)
1.2.4 ultra pure Water System (PALL, USA)
1.2.5 ultrasonic cleaning machine (Kunshan ultrasonic Instrument Co., ltd., KQ-100)
1.2.6 precision analytical balance (MettlerAE-100)
2. Method of producing a composite material
2.1 sample treatment
Pulverizing functional red rice sample (not less than 80 mesh) and mixing thoroughly. Accurately weighing 400.0-600.0mg of sample in a 50ml volumetric flask, adding 30ml of 75% ethanol (V/V), shaking uniformly, and performing ultrasonic treatment at room temperature for 20min (the working frequency is 40 KHz). Adding 75% ethanol to approximate scale, performing ultrasonic treatment for 10min, cooling to room temperature, and diluting to 50ml with 75% ethanol. Centrifuge at 3500 rpm for 10min. Taking the supernatant, passing through a 0.45 mu m pore diameter microporous filter membrane, and waiting for sample injection of the filtrate.
2.2 preparation of acid Monacolin K Standard
Weighing 4mg of Monacolin K (lactone) standard substance, fixing the volume to 100ml by using 0.2M sodium hydroxide solution, carrying out ultrasonic transformation for 1 hour at 50 ℃, cooling to room temperature, and then placing for 3 hours in a dark place for use. And calculating the conversion rate according to the chromatographic peak areas of the acid form Monacolin K and the residual lactone Monacolin K after the conversion. The prepared acid form Monacolin K is utilized to accurately determine the nature and quantity of the acid form Monacolin K in the sample.
2.3 chromatographic conditions
And (3) chromatographic column: c 18 Column 4.6X 250mm5 μm
Column temperature: at room temperature
Diode array detector: scanning at 200-350nm and processing data of chromatogram at 238nm
Mobile phase: methanol, water, phosphoric acid = 385: 115: 0.14 (V: V)
Flow rate: 1.0ml/min
Sample introduction amount: 20 μ l
2.4 map analysis
And (3) sampling 20 mu l of the treated sample extracting solution, detecting by a diode array detector to obtain a spectrum, and then determining the spectrum by using the retention time of standard Monacolin K (lactone and acid type) and the characteristic absorption spectrum of the Monacolin compound. And comparing the sum of the peak areas of the Monacolin components in the sample with the peak area of a standard Monacolin K (lactone or acid) chromatographic spectrum by taking a chromatogram under the wavelength of 238nm as a quantitative basis.
2.5 formula for calculation of results
In the formula: total amount of Monacolin compounds in X-form, mg/g
h 1 The sum of the peak areas of the separated component chromatograms with characteristic absorption spectra of the Monacolin-type compounds.
c-Standard Monacolin K (lactone type or acid type) solution concentration, mg/ml
50-sample constant volume, ml
h 2 Peak area of MonacolinK (lactone type or acid type)
m-sample weighing, g
3. Results of the experiment
3.1 investigation of chromatographic separation Effect
The separation of standard Monacolin K (lactone and acid type) under the above experimental conditions is shown in FIG. 1, and the separation of Monacolin type compounds of a certain red rice sample is shown in FIG. 2.
As can be seen from FIG. 1, the lactone form of Monacolin K is well separated from the ring-opened acid form of Monacolin K under the above-mentioned experimental conditions.
As can be seen from FIG. 2, under the above test conditions, the various Monacolin compounds in the red yeast samples were well separated. The diode array detector gives the instantaneous ultraviolet absorption spectrum of all separated component chromatograms. The spectra with the characteristics of the Monacolin compounds (one absorption peak at the wavelength of 230, 238 and 246nm and the maximum at the wavelength of 238 nm) are picked out, and the chromatographic peaks corresponding to the characteristic spectra in the chromatogram outflow curve chart are the Monacolin compounds.
3.2 investigation of Linear relationship and minimum detection Limit
The prepared standard solutions with concentrations of 0.1, 1, 10, 30, 75, 150, 300. Mu.g/ml MonacolinK (lactone type) were subjected to sample injection under the above-mentioned chromatographic conditions, and the peak area was plotted against the concentration as a standard curve, and the results are shown in FIG. 3. The linear regression equation and the correlation coefficient are respectively as follows: y =66084x-16840,R 2 =0.9999. Indicating a good linear relationship at this concentration.
When the concentration of Monacolin K is 0.1 mu g/ml, the chromatographic peak of Monacolin K is slightly more than 2 times of noise on a chromatographic outflow curve chart, so the lowest detection amount of the method is 0.1 mu g/ml (2 ng). From this standard curve, the optimal linear range of the method is 0.1-300 μ g/ml.
3.3 method parallelism precision test
The same homogeneous sample was divided into 5 portions and the experiment was performed in parallel starting from the previous treatment step, and the results of the measurement of the 5 portions are shown in table 1.
TABLE 1 measurement results of parallelism precision
| Serial number | Monacolin compound assay Determine the result (g/100g) | Mean value of | RSD |
| 1 2 3 | 0.294 0.296 0.293 | 0.294 | 0.002 |
| 4 5 | 0.292 0.296 |
The result shows that the method has good parallelism precision.
3.4 method repeatability precision test
The same homogeneous sample was tested once a day under the same experimental conditions starting from the sample pretreatment. The measurement was continued for 5 days, and the results are shown in Table 2.
TABLE 2 measurement of repeatability precision
| Serial number | Monacolin compound assay As a result, the (g/100g) | Mean value of | RSD |
| 1 2 3 4 5 | 0.41 0.43 0.42 0.42 0.44 | 0.424 | 2.69％ |
The result shows that the method has good repeatability and precision.
3.5 method recovery test
The sample was weighed exactly 10 parts, 5 of which were each added to a standard Monacolin K. The Monacolin K content in 10 samples was determined from the sample pretreatment. The results are as follows:
TABLE 3 determination of the recovery
| N Value of | In the sample Monacolin K Content mg | Adding into Quantity of mg | Detection of MonacolinK Content (wt.) mg | Recovery rate ％ | Mean value of |
| 1 2 3 4 5 | 0.64 0.71 0.71 0.69 0.65 | 2.0 2.0 2.0 2.0 2.0 | 2.60 2.64 2.70 2.64 2.73 | 98.3 96.5 99.3 97.8 97.9 | 97.96％ |
Table 3 shows that this method has good accuracy.
3.6 Determination of Monacolin compound content in 5 samples
Taking 5 red yeast samples respectively, measuring the content of the Monacolin compound by the detection method, wherein the result is as follows:
TABLE 4 measurement results of Monacolin compound content in samples
| Serial number | Sample name | Repeat the assay Number of times | Monacolin compound assay Results (g/100g) |
| 1 2 3 4 5 | XX Monascus sample
Article 1
XX |
6 6 6 6 6 | 1.02±0.02 0.80±0.01 0.99±0.02 1.20±0.11 0.45±0.10 |
As can be seen from Table 4, the method gives good results in practical applications.
4. Discussion of the related Art
4.1 the functional red yeast rice fermentation product contains various Monacolin compounds, mainly lactone type and acid type Monacolin K, the diode array detector can give all separated components of the chromatogram outflow instant ultraviolet absorption spectrum, the method can clearly reflect the separation condition of the Monacolin compounds which have the same ultraviolet absorption spectrum with the Monacolin K on the chromatogram outflow curve chart (see figure 2).
4.2 lactone type Monacolin K is commercially available. Since the acid form of Monacolin K is unstable, no standard substance is currently on the market. The standard lactone type Monacolin K can be conveniently converted into acid form by utilizing the conditions provided by the method. The conversion rate can be accurately obtained by using the ratio of peak areas of chromatographic peaks of acid form Monacolin K and lactone form Monacolin K after conversion, and the lactone form Monacolin K and the acid form Monacolin K in the sample can be accurately quantified.
4.3 Using a diode array detector, an instantaneous UV absorption spectrum scan of the chromatogram effluent can be performed on all separated components. Therefore, the method can simultaneously utilize the characteristic absorption spectrum of the Monacolin K for qualitative determination besides the Monacolin K retention time determination. This makes the qualitative analysis more reliable than the previous ultraviolet detector which can only use retention time for qualitative analysis.
4.4Monacolin compounds all have physiological activities similar to Monacolin K, the total amount of the Monacolin compounds in a sample can be obtained by adding peak areas of the components and quantifying the components by using standard lactone type Monacolin K, although errors exist due to the problem of detector response, the method is effective under the condition that the Monacolin compound standard substance is lacked at present. And because various Monacolin compounds in the sample are mainly in lactone type and acid type Monacolin K (see figure 2), the two compounds can be accurately quantified by using the method, and the content of other Monacolin compounds is very little, so the method has higher accuracy in measuring the total amount of the Monacolin compounds in the functional red yeast sample.
Claims (1)
1. A method for monitoring the content of Monacolin compounds in functional red yeast rice comprises the following steps:
(1) And a sample pretreatment step:
crushing a red yeast sample to be more than or equal to 80 meshes, and fully and uniformly mixing; accurately weighing 400.0-600.0mg of sample in a 50ml volumetric flask, adding 30ml of 75% ethanol by volume, shaking up, and performing ultrasonic treatment at the working frequency of 40KHz for 20min at room temperature; adding 75% ethanol to approximate scale, performing ultrasonic treatment for 10min, cooling to room temperature, and diluting to 50ml with 75% ethanol; centrifuging at 3500 rpm for 10min; taking supernatant fluid, passing through a 0.45 mu m pore diameter microporous filter membrane, and waiting for sample injection of filtrate;
(2) The preparation method of the acid form Monacolin K standard sample comprises the following steps:
weighing lactone type Monacolin K standard substance 4mg, fixing volume to 100ml with 0.2M sodium hydroxide solution, performing ultrasonic transformation at 50 deg.C for 1 hr, cooling to room temperature, and standing in dark for 3 hr; calculating the conversion rate according to the chromatographic peak areas of the converted acid type Monacolin K and the residual lactone type Monacolin K, and accurately determining the acid type Monacolin K in the sample by using the prepared acid type Monacolin K;
(3) And a chromatographic sample injection analysis step:
taking the filtrate filtered by the microporous filtration membrane to enter a liquid chromatograph, wherein the chromatographic conditions of the chromatograph are as follows: a chromatographic column: c 18 Column, 4.6X 250mm,5 μm; column temperature: room temperature; diode array detector: scanning at 200-350nm, and processing data of chromatogram at 238 nm; the volume ratio of the mobile phase is as follows: methanol, water, phosphoric acid = 385: 115: 0.14; flow rate: 1.0ml/min; sample introduction amount: 20 mu l of the mixture;
(4) And the step of map analysis and result calculation:
finding component peaks which have the same ultraviolet absorption spectrum with standard Monacolin K on a chromatogram outflow curve chart, namely Monacolin compounds, adding the peak areas of the components, comparing the peak areas with the chromatographic peak area of the standard Monacolin K, and calculating the total amount of the Monacolin compounds in the sample;
the resulting calculation formula is:
in the formula: x is the total amount of Monacolin compounds in the sample, mg/g
h 1 Is the sum of the chromatographic peak areas of separated components with the characteristic absorption spectrum of the Monacolin compound
c is the concentration of standard lactone type or acid type Monacolin K solution, mg/ml
50 is the volume of the sample with constant volume, ml
h 2 Peak area for lactone or acid form of MonacolinK
m is the sample weighing amount, g.
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| CN107677745A (en) * | 2017-09-29 | 2018-02-09 | 广西壮族自治区中医药研究院 | The quality determining method of Desmodium styracifolium extractive of general flavone |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240229A (en) * | 1999-07-23 | 2000-01-05 | 张军 | Process for preparing lovastatin-containing red koji mold body |
| US20040081663A1 (en) * | 2002-10-25 | 2004-04-29 | Chun-Min Chang | Pharmaceutical composition for treatment and prevention of cancer and the preparation thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1240229A (en) * | 1999-07-23 | 2000-01-05 | 张军 | Process for preparing lovastatin-containing red koji mold body |
| US20040081663A1 (en) * | 2002-10-25 | 2004-04-29 | Chun-Min Chang | Pharmaceutical composition for treatment and prevention of cancer and the preparation thereof |
Non-Patent Citations (2)
| Title |
|---|
| 紫外分光光度法测定红曲中酸式Lovastatin的含量. 文镜等.中国食品添加剂，第一期. 2002 * |
| 高效液相色谱法测定功能性红曲中洛伐他汀含量. 夏明等.药物分析杂志，第23卷第4期. 2003 * |
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