CN109061023B - Method for simultaneously separating and detecting contents of two dihydrochalcones in feed - Google Patents
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Abstract
The invention discloses a method for simultaneously separating and detecting the contents of two dihydrochalcones in feed, wherein the two dihydrochalcones are neohesperidin dihydrochalcone and naringin dihydrochalcone, and 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 (3) carrying out result analysis, wherein the method establishes a solid phase extraction-high performance liquid chromatography method of neohesperidin dihydrochalcone (NHDC) and Naringin dihydrochalcone (Naringin DC) in the feed.
Description
Technical Field
The invention relates to the field of feeds, in particular to a method for detecting the content of dihydrochalcone sweeteners, and specifically relates to a method for simultaneously separating and detecting solid-phase extraction-high performance liquid chromatography of neohesperidin dihydrochalcone and naringin dihydrochalcone in feeds.
Background
The dihydrochalcone derivative has the advantages of high sweetness, long duration, good stability and the like, and has good application in the feed industry. The compound premix can be used as a flavoring agent to be added into feed to generate a lasting fresh sweet effect, can play a synergistic effect by being compounded with other sweetening agents, can increase the appetite of piglets, promote the growth, improve the postpartum feeding of sows and shorten the postpartum recovery time. In addition, due to the excellent bitter taste masking and flavoring effects, the flavor and palatability of the feed can be greatly improved, and the bitter taste brought by adding medicaments or sweeteners such as saccharin, stevioside and the like into the feed can be masked. New hesperidin dihydrochalcone has been approved by European Union regulations (EU) 2015/264 to be added as a flavoring agent to feeds for fish, sheep, dogs, calves and certain types of pigs, and Chinese feed additive safety use Specification (revised 2017) allows the new hesperidin dihydrochalcone to be used as a pig feed sweetener, and the maximum limit of the new hesperidin dihydrochalcone is not more than 35 mg/kg.
At present, a method for detecting naringin dihydrochalcone is not reported, and methods for determining the naringin dihydrochalcone mainly comprise a high performance liquid chromatography (HP L C), a high performance liquid chromatography-tandem mass spectrometry (HP L C-MS/MS), a Capillary Zone Electrophoresis (CZE), an electrochemical sensor method and the like.
Disclosure of Invention
The invention aims to provide a method for simultaneously separating and detecting the contents of two dihydrochalcones in feed, which adopts the following technical scheme for realizing the aim:
the method is a method for simultaneously separating and detecting the contents of two dihydrochalcones in feed, and is mainly characterized in that the two dihydrochalcones are neohesperidin dihydrochalcone and naringin dihydrochalcone, and the detection method comprises the following steps:
the invention discloses a method for simultaneously separating and detecting the contents of two dihydrochalcones in feed, which comprises the following steps:
(1) preparing mixed standard stock solutions and mixed standard working solutions, wherein the mixed standard stock solutions are 980 mg/L mixed standard stock solutions, and the mixed standard working solutions are series standard working solutions with the concentrations of 0.196 mg/L, 0.490 mg/L, 0.980 mg/L, 4.90 mg/L, 9.80 mg/L and 49.0 mg/L prepared from the standard stock solutions of dihydrochalcone by a stepwise dilution method by using 50% methanol solutions;
(2) preparing a sample solution to be detected, namely adding 70 m L methanol solution into a feed sample, placing the feed sample into an ultrasonic oscillator for ultrasonic extraction for 30 min, transferring the feed sample into a 100 m L volumetric flask, fixing the volume to a scale mark by using methanol, uniformly mixing, centrifuging the extracting solution for 3min at 10000 r/min, taking 10 m L of supernatant into a 50 m L heart-shaped flask, spinning the supernatant into a nearly dry state at 40 ℃ on a rotary evaporator, carrying out vortex dissolution twice by using 2 m L50% methanol solution, transferring the solution into a 50 m L centrifugal tube, adding 8m L pure water, centrifuging for 3min at 10000 r/min, purifying the solution by using an H L B solid phase extraction column, blowing purified liquid nitrogen to 0.5 m L, adding 50% methanol solution to 1.0 m L, uniformly mixing, carrying out volume fixing by using a nylon 66 organic filter membrane, and filtering the filtrate for analysis.
(3) The instrument is a high performance liquid chromatograph, the detector is a photodiode array detector, the chromatographic column is a reversed phase C18 column, the column temperature is 35 +/-1 ℃, the detection wavelength is 282nm, the mobile phase A is methanol, the mobile phase B is pure water, the elution gradient program is 0-15.0 min, 43 percent A, 15.0-15.5 min, 43-90 percent A, 15.5-20.0 min, 90 percent A, 20.0-20.5 min, 90-43 percent A, 20.5-25.0 min, the flow rate of 43 percent A is 1.0 m L/min, and the sample injection amount is 25 mu L.
(4) Drawing a standard curve: and (3) injecting the series mixed standard working solution of the two dihydrochalcone sweeteners into a high performance liquid chromatograph, carrying out gradient 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, carrying out gradient elution and detection under the chromatographic condition obtained in the step (3), measuring the peak area of each target object in the filtrate, carrying out qualitative determination by retention time, and quantitatively calculating the content of each neohesperidin dihydrochalcone and naringin dihydrochalcone 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 detecting the content of dihydrochalcone sweeteners in feed, and considers that the maximum absorption wavelengths of neohesperidin dihydrochalcone and naringin dihydrochalcone are almost the same, a C18 column is selected as a fixed phase, and the composition and the proportion of a mobile phase are continuously optimized, so that the chromatographic conditions suitable for separating the content of the neohesperidin dihydrochalcone and the content of the naringin dihydrochalcone are obtained through research, all objects can be completely separated, and the optimal peak type and the sensitivity are obtained simultaneously.
2. The invention adopts a series of operations to ensure that the detection method has extremely high detection sensitivity to meet the requirement of adding neohesperidin dihydrochalcone and naringin dihydrochalcone in feed of feed enterprises, and comprises the steps of changing a preparation solution of a standard solution from a methanol solution to a 50% methanol solution to reduce the influence of a solvent effect in order to realize larger sample volume to ensure high sensitivity; meanwhile, weighing the sample by using a larger feed sample; in addition, a concentration method is adopted, so that the detection sensitivity is improved by 10 times.
3. The invention adopts the solid phase extraction method to purify complex feed samples, effectively avoids the introduction of more interference components, has strong anti-interference capability, and is particularly important for detecting low-content dihydrochalcone sweetener substances in complex matrixes.
4. The invention has extremely high detection sensitivity, the limit of quantification is as low as 0.016mg/kg, which is far lower than the maximum limit requirement (35 mg/kg) of a detection method (the limit of quantification is 0.8 mg/kg) adopted by European Union and related regulations on the dihydrochalcone sweetener, and simultaneously, the invention has strong anti-interference capability, and can completely meet the daily monitoring and supervision requirements of the dihydrochalcone sweetener in the feed.
5. 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. Meanwhile, the defects of poor stability, poor reproducibility and the like of a capillary electrophoresis method and an electrochemical sensor can be overcome.
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FIG. 1 is a mixed standard solution high performance liquid chromatography separation chart of the simultaneous separation and detection method of the contents of neohesperidin dihydrochalcone and naringin dihydrochalcone in the feed.
Detailed Description
The present invention will be described in further detail with reference to specific examples. The present invention is now described in detail and specific procedures for implementing the present invention on the premise of the technology 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 methanol: and (4) carrying out chromatographic purification.
1.2H L B solid phase extraction column 60 mg/3 m L.
1.3, standard substance: neohesperidin dihydrochalcone (NHDC, purity not less than 98.0%, Shanghai Michelin, China); naringin dihydrochalcone (Naringin DC, purity greater than or equal to 98.0%, Aladdin USA). .
1.4 preparation of standard stock solution, namely accurately weighing 0.1000g of each of neohesperidin dihydrochalcone and naringin dihydrochalcone standard products, dissolving the new hesperidin dihydrochalcone and the naringin dihydrochalcone standard products by using a methanol solution, and fixing the volume to 100 m L to prepare the standard stock solution with the concentration of 980 mg/L, and storing the standard stock solution at 0-4 ℃ for 3 months.
1.5 preparation of standard working solution, namely preparing a series of standard working solutions with the concentrations of 0.196 mg/L, 0.490 mg/L, 0.980 mg/L, 4.90 mg/L, 9.80 mg/L and 49.0 mg/L from standard stock solutions of neohesperidin dihydrochalcone and naringin dihydrochalcone by a stepwise dilution method, and storing all the standard working solutions in a refrigerator at the temperature of 0-4 ℃ for 1 month.
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 centrifuge: the rotating speed is not lower than 10000 r/min; .
2.6 organic filter membranes of nylon 66: 0.45 μm.
3 method
3.1 high Performance liquid chromatography conditions
a) The chromatographic column is an XB-C18 column with the diameter of 5 mu m and the diameter of 150 mm of × 4.6.6 mm;
b) the mobile phase A is methanol, the mobile phase B is pure water, the elution gradient program is 0.0-15.0 min, 43 percent of A, 15.0-15.5 min, 43-90 percent of A, 15.5-20.0 min, 90 percent of A, 20.0-20.5 min, 90-43 percent of A, 20.5-25.0 min, and the flow rate of 43 percent of A is 1.0 m L/min;
c) the flow rate is 1.0 m L/min;
d) column temperature: 35 ℃;
e) the sample injection amount is 25 mu L;
f) detection conditions of the photodiode array detector: detection wavelength of 282nm
3.2 Standard Curve plotting
The mixed standard working solution (1.5) is taken respectively, chromatographic determination is carried out according to chromatographic conditions of 3.1, and a standard curve is drawn by linear regression of the peak area (Y) of each analyte to the corresponding mass concentration (X, mg/L), so as to obtain a linear regression equation.
4 sample testing procedure
4.1 sample pretreatment
Weighing 10 g (accurate to 0.01 g) of a feed sample in a 100 m L conical flask with a plug, adding 70 m L methanol solution, placing the feed sample in an ultrasonic oscillator for ultrasonic extraction for 30 min, transferring the feed sample to a 100 m L0 volumetric flask, fixing the volume to a scale mark by using methanol, uniformly mixing, centrifuging the extracting solution at 10000 r/min for 3min, taking 10 m L of supernatant in a 50 m L2 chicken heart flask, rotating the supernatant on a rotary evaporator at 40 ℃ until the supernatant is nearly dry, dissolving the supernatant by using 2 m L% methanol solution twice in a vortex, transferring the supernatant to a 50 m L centrifugal tube, adding 8m L5 pure water, centrifuging the supernatant for 3min at 10000 r/min, purifying, rinsing the small column by using 3m L methanol and 3m L B, transferring the solution to the small column H L B, keeping the flow rate of the flowing-2 d/min, after the flowing out of the column liquid completely, rinsing the small column by using 5m L% methanol solution and 3m L% methanol, fixing the volume of H L B small column, transferring the flowing-free solution to 8536% of nylon, uniformly mixing, adding 890.36% methanol, eluting, and filtering the eluting solution, and filtering the eluting by adding 66% of filter membrane for uniform filtration and analyzing.
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 contents of neohesperidin dihydrochalcone and naringin dihydrochalcone in the sample were calculated by the following formula (1):
X＝
（1）
in the formula:
X-the content of neohesperidin dihydrochalcone and naringin dihydrochalcone in milligrams per kilogram (mg/kg) in the sample;
C i -the sample concentration of the sample solution in milligrams per liter (mg/L);
V-sample volumetric volume in milliliters (m L);
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 linearity, detection limit and quantitative limit, namely preparing two series of mixed standard working solutions with the concentration of the dihydrochalcone between 0.196 mg/L and 49.0 mg/L, performing linear regression on the concentration by peak area, wherein a linear equation, a correlation coefficient, the detection limit and the quantitative limit are shown in a table 1rThe total content of the dihydrochalcone is more than 0.999, the quantitative limits are respectively 0.011 mg/kg and 0.016mg/kg, and the quantitative limit of the method can completely meet the detection requirement of the dihydrochalcone in the feed.
y is peak area, x is mass concentration, mg/L.
6.2 recovery and precision: under the optimized detection condition, a feed sample is taken to carry out a standard adding recovery rate test, the standard adding levels are respectively 0.98 mg/kg, 4.7 mg/kg and 9.80 mg/kg, each level is repeatedly analyzed for 3 times, and the result is shown in table 2. As can be seen from the table 2, the range of the standard recovery rate of the method is 86.2-105.0%, and the range of the relative standard deviation RSD is 1.0-6.3%, and the result shows that the method is suitable for daily analysis and detection of two dihydrochalcones in the feed.
Finally, the above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and although the present invention has been described in detail with reference to the embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made to the technical solution of the present invention without departing from the spirit and scope of the technical solution of the present invention, which should be covered by the claims of the present invention.
Claims (6)
1. The method for simultaneously separating and detecting the contents of two dihydrochalcones in the feed is characterized in that the two dihydrochalcones are neohesperidin dihydrochalcone and naringin dihydrochalcone; the detection method comprises the following steps:
(1) preparing mixed standard stock solutions and mixed standard working solutions, wherein the mixed standard stock solutions are 980 mg/L mixed standard stock solutions, and the mixed standard working solutions are series standard working solutions with the concentrations of 0.196 mg/L, 0.490 mg/L, 0.980 mg/L, 4.90 mg/L, 9.80 mg/L and 49.0 mg/L prepared from the standard stock solutions of dihydrochalcone by a stepwise dilution method by using 50% methanol solutions;
(2) preparing a sample solution to be detected, namely adding 70 m L methanol solution into a feed sample, placing the feed sample into an ultrasonic oscillator, carrying out ultrasonic extraction for 30 min, transferring the feed sample into a 100 m L volumetric flask, fixing the volume to a scale mark by using methanol, uniformly mixing, centrifuging the extract for 3min at 10000 r/min, taking 10 m L of supernatant into a 50 m L heart-shaped flask, spinning the supernatant on a rotary evaporator at 40 ℃ to be nearly dry, carrying out vortex dissolution twice by using 2 m L50% methanol solution, transferring the dissolved solution into a 50 m L centrifugal tube, adding 8m L pure water, centrifuging the solution for 3min at 10000 r/min, purifying the solution by using an H L B solid phase extraction column, purifying liquid nitrogen to be blown to 0.5 m L, adding 50% methanol solution to 1.0 m L, uniformly mixing, carrying out volume fixing by using a nylon 66 organic filter membrane, and filtering the filtrate for analysis;
(3) the used instrument is a high performance liquid chromatograph, the detector is a photodiode array detector, the chromatographic column is a reversed phase C18 column, the column temperature is 35 +/-1 ℃, the detection wavelength is 282nm, the mobile phase A is methanol, the mobile phase B is pure water, the elution gradient program is 0-15.0 min, 43 percent A, 15.0-15.5 min, 43-90 percent A, 15.5-20.0 min, 90 percent A, 20.0-20.5 min, 90-43 percent A, 20.5-25.0 min, 43 percent A, the flow rate is 1.0 m L/min, and the sample introduction amount is 25 mu L;
(4) drawing a standard curve: injecting a series of mixed standard working solutions of the two dihydrochalcone sweeteners into a high performance liquid chromatograph, performing gradient 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, carrying out gradient elution and detection under the chromatographic condition of the step (3), measuring peak areas of all target objects in the filtrate, carrying out qualitative determination by retention time, and quantitatively calculating the contents of the neohesperidin dihydrochalcone and the naringin dihydrochalcone in the sample to be detected according to the standard curve prepared in the step (4).
2. The method for simultaneously separating and detecting the content of two dihydrochalcones in the feed according to claim 1, wherein the preparation of the mixed standard stock solution in the step (1) comprises the specific steps of accurately weighing 0.1000g of each of neohesperidin dihydrochalcone and naringin dihydrochalcone standard products, dissolving the neohesperidin dihydrochalcone and the naringin dihydrochalcone standard products by using a methanol solution, fixing the volume to 100 m L, and preparing standard stock solutions with the concentrations of 980 mg/L, wherein the preparation of the mixed standard working solution in the step (1) comprises the specific steps of preparing the standard stock solutions of neohesperidin dihydrochalcone and naringin dihydrochalcone by using a 50% methanol solution by using a stepwise dilution method to prepare series standard working solutions with the concentrations of 0.196 mg/L, 0.490 mg/L, 0.980 mg/L, 4.90 mg/L, 9.80 mg/L and 49.0 mg/L, and placing all the standard stock solutions and the standard working solutions in a refrigerator to be stored at the temperature of 0-4 ℃.
3. The method for simultaneously separating and detecting the content of two dihydrochalcones in the feed according to claim 1, wherein the step (2) of preparing the sample solution to be detected comprises the following specific steps:
weighing 10 g of feed sample, accurately weighing to 0.01 g, placing the feed sample in a 100 m L conical flask with a plug, adding 70 m L methanol solution, placing the feed sample in an ultrasonic oscillator for ultrasonic extraction for 30 min, transferring the feed sample to a 100 m L0 volumetric flask, fixing the volume to a scale mark by using methanol, uniformly mixing, centrifuging the extracting solution at 10000 r/min for 3min, taking 10 m L of supernatant in a 50 m L2 chicken heart flask, rotating the supernatant on a rotary evaporator at 40 ℃ until the supernatant is nearly dry, performing vortex dissolution by using 2 m L% methanol solution twice, transferring the supernatant to a 50 m L centrifugal tube, adding 8m L5 pure water, centrifuging the supernatant for 3min at 10000 r/min, purifying, rinsing the H L B column by using 3m L methanol and 3m L% methanol sequentially, transferring the solution to the H L B column, keeping the flow rate of the flowing-out liquid for 1-2 d/min, after the column liquid completely flows out, rinsing the 5m L% methanol solution, fixing the volume by using 60 m L%, uniformly mixing, adding 890.30% methanol, eluting by using a filter membrane to obtain an organic elution solution, and filtering the solution, and uniformly mixing.
4. The method for simultaneously separating and detecting the content of two dihydrochalcones in the feed according to claim 1, wherein the reversed-phase C18 chromatographic column in the step (3) has a specification of 150 mm × 4.6.6 mm inner diameter and a particle size of 5 μm.
5. The method for simultaneously separating and detecting the content of two dihydrochalcones in the feed according to claim 1, wherein the coefficient of the standard curve in the step (4) is not less than 0.999.
6. The method for simultaneously separating and detecting the content of two dihydrochalcones in the feed according to claim 1, wherein the feed is a pig feed or a fish feed.
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