CN112461975A - Method for detecting coenzyme content in feed additive - Google Patents
Method for detecting coenzyme content in feed additive Download PDFInfo
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- CN112461975A CN112461975A CN202011387282.7A CN202011387282A CN112461975A CN 112461975 A CN112461975 A CN 112461975A CN 202011387282 A CN202011387282 A CN 202011387282A CN 112461975 A CN112461975 A CN 112461975A
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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Abstract
The invention discloses a method for detecting coenzyme content in a feed additive, wherein the coenzyme is pyrroloquinoline quinone disodium; the detection method is high performance liquid chromatography. The method comprises the following steps: (1) preparing a mixed standard stock solution and a mixed standard working solution; (2) preparing a sample solution to be detected; (3) high performance liquid chromatography analysis conditions; (4) establishing a standard working curve; (5) and (6) analyzing results. The method establishes a high performance liquid chromatography detection method for the content of the pyrroloquinoline quinine disodium serving as the feed additive. The method makes up the blank of the detection method for the content of the pyrroloquinoline quinine disodium of the feed additive, is simple, convenient and quick, has good reproducibility, and is suitable for daily detection of the content of the pyrroloquinoline quinine disodium of the feed additive.
Description
Technical Field
The invention relates to the field of feeds, in particular to a method for detecting the content of pyrroloquinoline quinine disodium, and specifically relates to a high performance liquid chromatography detection method of pyrroloquinoline quinine disodium as a feed additive.
Background
Pyrroloquinoline quinone (PQQ) is another oxidoreductase coenzyme found in microorganisms following nicotinamide and riboflavin, and is widely present in biological tissues of prokaryotes, plants, and mammals. PQQ has multiple functions of resisting oxidation, promoting nerve growth factor regeneration and the like. In feed applications, pyrroloquinoline quinone disodium salt (PQQ-2Na) is the most commonly used form of pyrroloquinoline quinone (PQQ). Relevant researches show that the pyrroloquinoline quinone disodium salt has strong antioxidant capacity, can regulate the antioxidant capacity and the metabolic capacity of a laying hen body, promotes the early development and growth capacity of laying hens, particularly newborn laying hens, and increases the yield and the survival rate of piglets and mice, so that the pyrroloquinoline quinone disodium salt has a wide application prospect as a feed additive in feeds. At present, the detection of pyrroloquinoline quinone disodium salt in the feed additive is not reported.
Disclosure of Invention
The invention aims to provide a high performance liquid chromatography detection method of a feed additive pyrroloquinoline quinine disodium, which is used for making up and solving the defect that no detection method of the content of the feed additive pyrroloquinoline quinine disodium exists at present, so that the method can accurately analyze the content of the feed additive pyrroloquinoline quinine disodium.
In order to achieve the purpose, the invention adopts the following technical scheme:
the method is a method capable of detecting the coenzyme content in the feed additive, and is mainly characterized in that the coenzyme is pyrroloquinoline quinone disodium, and the method for detecting the coenzyme content in the feed additive comprises the following steps:
(1) preparing a mixed standard stock solution and a mixed standard working solution, wherein the standard stock solution is 1.30 mg/mL, and the standard working solution is a series of standard working solutions with the concentrations of 0.2 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 9.8 mg/L and 49.0 mg/L, which are prepared from the standard stock solution of pyrroloquinoline quinone disodium by adopting a stepwise dilution method;
(2) preparing a sample solution to be tested: adding 8mL of diluent into a 25 mL colorimetric tube with a plug, placing the feed additive sample into an ultrasonic oscillator for ultrasonic extraction for 20 min, fixing the volume to a scale mark by using the diluent, uniformly mixing, filtering by using a water-phase filter membrane, and analyzing the filtrate;
(3) the used instrument is a high performance liquid chromatograph, and the detector is a photodiode array detector; the chromatographic column is a reversed phase C18 column, the temperature of the column is 35 +/-1 ℃, and the detection wavelength is 249 nm; mobile phase a was acetonitrile, mobile phase: acetonitrile (a) -mobile phase salt solution (B) =40/60 isocratic elution; elution time: 12 min; the flow rate is 1.0 mL/min; the sample size was 5. mu.L.
(4) Drawing a standard curve: and (3) injecting the series of mixed standard working solutions of pyrroloquinoline quinone disodium into a high performance liquid chromatograph, carrying out isocratic elution and detection under the chromatographic condition of the step (3), determining the nature by retention time, and drawing a standard curve according to the corresponding relation between the peak area size and the concentration of each concentration.
(5) And (4) analyzing results: and (3) injecting the filtrate obtained in the step (2) into a high performance liquid chromatograph, performing isocratic elution and detection under the chromatographic condition of the step (3), measuring peak areas of all target objects in the filtrate, performing qualitative determination by retention time, and quantitatively calculating the content of pyrroloquinoline quinone disodium in the sample to be measured according to the standard curve prepared in the step (4).
Compared with the prior art, the invention has the following outstanding advantages:
1. the invention fills the blank in the field of detection of the content of the pyrroloquinoline quinone disodium of the feed additive, and the prior art mainly aims at the fact that the pyrroloquinoline quinone in functional food, the feed additive and the functional food matrix are completely different, and a new technology is urgently needed to be established to meet the detection requirement of the pyrroloquinoline quinone disodium of the feed additive.
2. In the invention, a C18 column is selected as a stationary phase, and the finding that the pyrroloquinoline quinone disodium can not generate peaks when common mobile phases such as acetonitrile and water are used in daily life is carried out.
3. The analytical instrument used in the invention is a high performance liquid chromatograph equipped with a photodiode array detector, and is easier to popularize, popularize and apply compared with instruments with high manufacturing cost such as a liquid chromatograph-mass spectrometer.
The invention establishes the high performance liquid chromatography method for determining the pyrroloquinoline quinone disodium as the feed additive. The method is simple and rapid, has good reproducibility, is suitable for quantitative detection of pyrroloquinoline quinine disodium as a feed additive, and can provide technical support for feed additive production enterprises, feed additive supervision departments and import and export detection departments.
Drawings
FIG. 1 is a high performance liquid chromatography separation chart of a standard solution of pyrroloquinoline quinone disodium content in the feed additive of the present invention.
Detailed Description
The invention is described in further detail below with reference to the drawings of the detailed description of embodiments. The present invention is implemented on the premise of the technology of the present invention, and the detailed embodiments and specific operation procedures are given to illustrate the inventive aspects of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
1 reagents and materials
All reagents were analytically pure except where otherwise stated, and water was the secondary water specified in GB/T6682.
1.1 acetonitrile: and (4) carrying out chromatographic purification.
1.2 comparison products: pyrroloquinoline quinone disodium (PQQ-2Na, purity 86.5%) was supplied by Fujian Youbefu Biotech Co., Ltd.
1.3 solution preparation: diluting liquid: 1.13g of disodium hydrogen phosphate and 0.95g of sodium dihydrogen phosphate were weighed and dissolved in 500mL of pure water. Mobile phase salt solution: 3.87g of tetrabutylammonium bromide and 1.632g of potassium dihydrogen phosphate were weighed out and dissolved in 600mL of pure water. Preparation of a standard stock solution: 0.1501g of pyrroloquinoline quinone disodium reference substance is accurately weighed, dissolved by a diluent and fixed to 100 mL, and a standard stock solution with the concentration of 1.30 mg/mL is prepared. Preparation of standard working solution: the standard stock solution of pyrroloquinoline quinone disodium is diluted by a stepwise dilution method to prepare a series of standard working solutions with the concentrations of 0.2 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 9.8 mg/L and 49.0 mg/L by using a diluent. And storing all the standard stock solution and the standard working solution in a refrigerator at the temperature of 0-4 ℃.
2 instruments and apparatus
2.1 high performance liquid chromatograph: equipped with a diode array detector.
2.2 analytical balance: 0.0001 g of sensory quality and 0.01 g of sensory quality.
2.4 ultrasonic generator: the power is greater than 180W.
2.5 aqueous phase filtration membrane: 0.45 μm.
3 method
3.1 high Performance liquid chromatography conditions
a) A chromatographic column: XB-C18 column, 5 μm, 250 mm × 4.6 mm;
b) mobile phase: mobile phase: acetonitrile (a) -mobile phase salt solution (B) =40/60 isocratic elution; elution time: 12 min;
c) flow rate: 1.0 mL/min;
d) column temperature: 35 ℃;
e) sample introduction amount: 25 mu L of the solution;
f) detection conditions of the photodiode array detector: detection wavelength 249nm
3.2 Standard Curve plotting
The standard working solutions (1.3) were each subjected to chromatography under the chromatographic conditions of 3.1. And (5) performing linear regression on the corresponding mass concentration (X, mg/L) by using the peak area (Y) of each analyte to draw a standard curve to obtain a linear regression equation.
4 sample testing procedure
4.1 sample pretreatment
Weighing 0.1g (accurate to 0.0001 g) of feed additive sample into a 25 mL colorimetric tube with a plug, adding 8mL of diluent, placing the colorimetric tube in an ultrasonic oscillator for ultrasonic extraction for 20 min, fixing the volume to a scale mark by using the diluent, uniformly mixing, filtering by using an aqueous phase filter membrane, and allowing the filtrate to be used for analysis.
4.2 assay in test solution
The prepared sample solution was subjected to chromatography under the same chromatographic conditions, qualitative by retention time, and quantitative by external standard method.
5 presentation of the results of the analysis
The content of pyrroloquinoline quinone disodium in the sample was calculated by the following formula (1):
in the formula:
X-the content of pyrroloquinoline quinone disodium in the sample in percent (%);
C i -the sample concentration of the test solution in milligrams per liter (mg/L);
V-sample volumetric volume in milliliters (mL);
msample mass in grams (g).
Results are presented as the arithmetic mean of two independent measurements obtained under repetitive conditions, with three significant figures remaining.
6 methodology investigation including linearity, detection limit, quantitation limit, recovery, precision.
6.1 Linear, detection Limit, quantification Limit: preparing a series of mixed standard working solutions with the concentration of the pyrroloquinoline quinine disodium salt between 13.0 mg/L and 520 mg/L, performing linear regression on the concentration by using the peak area, and obtaining a linear equationThe correlation coefficient is shown in Table 1. The result shows that the pyrroloquinoline quinine disodium has good linear relation and correlation coefficient within 13.0-520 mg/LrIs 0.9997, and the method can completely meet the detection requirement of pyrroloquinoline quinone disodium in the feed additive.
TABLE 1 regression equation, correlation coefficient, Linear Range of pyrroloquinoline quinone disodium
| Components | Linear equation-Y=ax +b | Relevant coefficient-r | Linear range/(mg/L) |
| Pyrroloquinoline quinone disodium salt | Y=1.86×105 x-1590 | 0.9997 | 13.0 - 520 |
YPeak area;x: mass concentration, mg/L.
6.2 recovery and precision: under the optimized detection condition, a blank substrate yeast powder sample is taken to carry out a standard addition recovery rate test, the standard addition levels are 5.2%, 10.4% and 20.8% respectively, each level is repeatedly analyzed for 3 times, and the result is shown in table 2. As can be seen from Table 2, the standard recovery rate of the method is in the range of 101.7-102.2%, and the relative standard deviation RSD is in the range of 0.7-3.6%, and the result shows that the method is suitable for daily analysis and detection of pyrroloquinoline quinone disodium in the feed additive.
Table 2 feed additive sample standard recovery test results (n ═ 3)
6.3 stability: taking the pyrroloquinoline quinone disodium standard solutions with the mass concentrations of 13.0 mg/L, 130 mg/L and 520 mg/L within the standard curve range, placing the standard solutions at room temperature for 2 h, 4 h, 6 h, 8 h, 12 h and 2-6 days, and inspecting the daily and diurnal stability of the pyrroloquinoline quinone disodium standard solutions. Experimental results show that the precision of the daily stability of the low, medium and high quality pyrroloquinoline quinine disodium standard solution is 0.2-0.9%, 0.1-0.5% and 0.1-0.9%, and the precision of the daily stability is 0.2-1.3%, 0.1-0.8% and 0.1-1.1%, respectively. Therefore, the pyrroloquinoline quinine disodium is good in stability in the day and in the daytime, and is beneficial to the experiment.
Finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (5)
1. The method for detecting the coenzyme content in the feed additive is characterized in that the coenzyme is pyrroloquinoline quinone disodium; the detection method comprises the following steps:
(1) preparing a standard stock solution and a standard working solution, wherein the standard stock solution is 1.30 mg/mL, and the standard working solution is a series of standard working solutions with the concentrations of 0.2 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 9.8 mg/L and 49.0 mg/L, which are prepared from the standard stock solution of pyrroloquinoline quinone disodium by adopting a stepwise dilution method;
(2) preparing a sample solution to be tested: adding 8mL of diluent into a 25 mL colorimetric tube with a plug, placing the feed additive sample into an ultrasonic oscillator for ultrasonic extraction for 20 min, fixing the volume to a scale mark by using the diluent, uniformly mixing, filtering by using a water-phase filter membrane, and analyzing the filtrate;
(3) the used instrument is a high performance liquid chromatograph, and the detector is a photodiode array detector; the chromatographic column is a reversed phase C18 column, the temperature of the column is 35 +/-1 ℃, and the detection wavelength is 249 nm; mobile phase a was acetonitrile, mobile phase: acetonitrile (a) -mobile phase salt solution (B) =40/60 isocratic elution; elution time: 12 min; the flow rate is 1.0 mL/min; the sample injection amount is 5 mu L;
(4) drawing a standard curve: injecting the series of mixed standard working solutions of pyrroloquinoline quinone disodium into a high performance liquid chromatograph, carrying out isocratic elution and detection under the chromatographic condition of the step (3), determining the nature by retention time, and drawing a standard curve according to the corresponding relation between the peak area size and the concentration of each concentration;
(5) and (4) analyzing results: and (3) injecting the filtrate obtained in the step (2) into a high performance liquid chromatograph, performing isocratic elution and detection under the chromatographic condition of the step (3), measuring peak areas of all target objects in the filtrate, performing qualitative determination by retention time, and quantitatively calculating the content of pyrroloquinoline quinone disodium in the sample to be measured according to the standard curve prepared in the step (4).
2. The method for detecting the coenzyme content in the feed additive according to claim 1, wherein the preparation of the mixed standard stock solution in (1) comprises the following specific steps: weighing 1.13g of disodium hydrogen phosphate and 0.95g of sodium dihydrogen phosphate, dissolving in 500mL of pure water to prepare a diluent, accurately weighing 0.1501g of pyrroloquinoline quinine disodium reference substance, dissolving with the diluent and fixing the volume to 100 mL, and preparing a standard stock solution with the concentration of 1.30 mg/mL; (1) the preparation method of the mixed standard working solution comprises the following specific steps: preparing a series of standard working solutions with the concentrations of 0.2 mg/L, 0.5 mg/L, 1.0 mg/L, 5.0 mg/L, 9.8 mg/L and 49.0 mg/L from the standard stock solution of pyrroloquinoline quinone disodium by adopting a stepwise dilution method, and storing all the standard stock solution and the standard working solutions in a refrigerator at the temperature of 0-4 ℃.
3. The method for detecting the coenzyme content in the feed additive according to claim 1, wherein the preparation of the sample solution to be detected in (2) comprises the following steps: weighing 0.1g of feed sample, accurately weighing the feed sample to 0.0001 g, adding 8mL of diluent into a 25 mL colorimetric tube with a plug, placing the colorimetric tube in an ultrasonic oscillator for ultrasonic extraction for 20 min, fixing the volume to a scale mark by using the diluent, uniformly mixing, filtering by using an aqueous phase filter membrane, and allowing the filtrate to be used for analysis.
4. The method for detecting the coenzyme content in the feed additive according to claim 1, wherein the specification of the reversed phase C18 chromatographic column in (3) is 250 mm x 4.6 mm in inner diameter, and the particle size is 5 μm.
5. The method for detecting the coenzyme content in the feed additive according to claim 1, wherein the standard curve coefficient in (4) is not less than 0.999.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117471005A (en) * | 2023-10-26 | 2024-01-30 | 山东省食品药品检验研究院 | Method for detecting pyrroloquinoline quinone disodium salt in milk beverage |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102072942A (en) * | 2010-11-24 | 2011-05-25 | 江苏省原子医学研究所 | Analysis method for measuring pyrroloquinoline quinine content through ion pair chromatography |
| CN102323340A (en) * | 2011-06-09 | 2012-01-18 | 江苏省原子医学研究所 | Action of pyrro-quinoline quinone and amino acid neurotransmitters |
| US20120323009A1 (en) * | 2010-02-16 | 2012-12-20 | Mitsubishi Gas Chemical Company, Inc. | Production method of reduced pyrroloquinoline quinone |
| CN105334301A (en) * | 2015-11-27 | 2016-02-17 | 潍坊盛瑜药业有限公司 | Pyrrolo quinoline quinone (PQQ) disodium salt impurity separation and purification method |
| CN109085269A (en) * | 2018-08-15 | 2018-12-25 | 江苏省原子医学研究所 | The method of PQQ and Lys and Arg reflex action research |
| TW201930874A (en) * | 2018-01-12 | 2019-08-01 | 日商三菱瓦斯化學股份有限公司 | Analysis method |
-
2020
- 2020-12-02 CN CN202011387282.7A patent/CN112461975A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20120323009A1 (en) * | 2010-02-16 | 2012-12-20 | Mitsubishi Gas Chemical Company, Inc. | Production method of reduced pyrroloquinoline quinone |
| CN102072942A (en) * | 2010-11-24 | 2011-05-25 | 江苏省原子医学研究所 | Analysis method for measuring pyrroloquinoline quinine content through ion pair chromatography |
| CN102323340A (en) * | 2011-06-09 | 2012-01-18 | 江苏省原子医学研究所 | Action of pyrro-quinoline quinone and amino acid neurotransmitters |
| CN105334301A (en) * | 2015-11-27 | 2016-02-17 | 潍坊盛瑜药业有限公司 | Pyrrolo quinoline quinone (PQQ) disodium salt impurity separation and purification method |
| TW201930874A (en) * | 2018-01-12 | 2019-08-01 | 日商三菱瓦斯化學股份有限公司 | Analysis method |
| CN109085269A (en) * | 2018-08-15 | 2018-12-25 | 江苏省原子医学研究所 | The method of PQQ and Lys and Arg reflex action research |
Non-Patent Citations (4)
| Title |
|---|
| XINGQIN ZHOU 等: "Ion-Pair LC Analysis of Pyrroloquinoline Quinone in Neurotransmitter Amino Acid Incubations: Determination of Chemical Kinetics", 《CHROMATOGRAPHIA》 * |
| XUE-PENG YANG 等: "UPLC-DAD-MS/MS Method for Analysis of PQQ in Fermentation Broth", 《CHROMATOGRAPHIA》 * |
| 杨海锋 等: "高效液相色谱法测定抗氧化剂乙氧基喹啉含量", 《粮食与饲料工业》 * |
| 魏静远 等: "高效液相色谱法分析吡咯喹啉醌", 《生物技术通讯》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117471005A (en) * | 2023-10-26 | 2024-01-30 | 山东省食品药品检验研究院 | Method for detecting pyrroloquinoline quinone disodium salt in milk beverage |
| CN117471005B (en) * | 2023-10-26 | 2024-04-16 | 山东省食品药品检验研究院 | Method for detecting pyrroloquinoline quinone disodium salt in milk beverage |
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