CN111257495A - Method for detecting nitrate and nitrite - Google Patents
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- 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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- G01N30/02—Column chromatography
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Abstract
The invention relates to a method for detecting nitrate and nitrite in livestock meat and products thereof, which comprises the steps of sample pretreatment, standard curve preparation and content determination of a solution to be detected. By optimizing the pretreatment method and the instrument detection conditions, the detection method disclosed by the invention makes up for the defects of detection by a national standard method, has the advantages of simplicity in operation, short test period, low loss, high recovery rate, good precision and the like, can effectively reduce the interference of impurities on the detection of nitrate and nitrite, and is suitable for rapid determination of nitrate and nitrite in meat and meat products.
Description
Technical Field
The invention relates to the field of detection, in particular to a method for detecting nitrate and nitrite.
Background
Nitrate and nitrite can be used as color fixative and antiseptic to be added into meat product, which is helpful to improve meat color, inhibit growth and reproduction of microorganism, and prolong shelf life of meat product. However, nitrite can convert hemoglobin of human body into methemoglobin, so that blood loses oxygen carrying function, and has carcinogenic and teratogenic effects, and excessive amount of nitrite can even endanger life.
Only 4 kinds of nitrates and nitrites which are approved to be used in China include sodium nitrate, potassium nitrate, sodium nitrite and potassium nitrite, wherein the sodium nitrate and the sodium nitrite are widely applied. GB2760-2014 food additive use standard stipulates that the maximum use amount of nitrate in various cooked meat products such as cured meat products, sauced and marinated meat products, western meat products and the like is 0.5g/kg, and the residual amount is less than or equal to 30mg/kg (by NO)3 -A meter); the maximum usage amount of nitrite is 0.15g/kg, and the residual amount is less than or equal to 30mg/kg (by NO)2 -Meter). Because of the safety problem of nitrate and nitrite, people pay attention to how to measure and reduce the residual quantity of nitrate and nitrite, and therefore, the detection of the content of nitrate and nitrite in the livestock and poultry meat products has important significance.
At present, the detection methods of nitrate and nitrite in food mainly include ion chromatography, spectrophotometry, chemiluminescence, liquid chromatography, gas chromatography, and the like. Among them, ion chromatography is listed as one of the national standard inspection methods, and is widely applied to meat product detection due to its simple operation and stable recovery rate.
The current effective detection method GB5009.33-2016 is complex in pretreatment operation, long in time consumption, low in recovery rate and poor in precision. Therefore, a method for detecting nitrate and nitrite in livestock and poultry meat and products thereof with high recovery rate, good precision and accurate and reliable result is needed to be established.
Disclosure of Invention
The invention aims to provide a method for detecting nitrate and nitrite in livestock and poultry meat and products thereof, which has high recovery rate, good precision and accurate and reliable result.
The invention provides a method for detecting nitrate and nitrite in livestock meat and products thereof, which comprises the following steps:
(1) sample pretreatment: weighing a homogeneous sample of livestock and poultry meat, adding water for ultrasonic extraction, heating in a water bath, taking out, cooling to room temperature, adding an organic solvent, fully mixing, standing, centrifuging, and taking supernatant to sequentially pass through a 0.22 mu m filter membrane, an RP column and a Na column for later use;
(2) and (3) preparing a standard curve: respectively injecting the standard series working solution of nitrate ions and nitrite ions into an ion chromatograph to obtain standard working solution chromatograms with various concentrations, measuring corresponding peak areas, and drawing standard curves of the nitrate ions and the nitrite ions by taking the mass concentrations of the nitrate ions and the nitrite ions as horizontal coordinates and the peak areas as vertical coordinates;
(3) and (3) content determination of the solution to be detected: injecting the blank solution and the solution to be detected into an ion chromatograph to obtain peak areas of the blank solution and the sample solution, and calculating the content of nitrate and nitrite in the solution to be detected according to a standard curve;
wherein, the ion chromatography conditions in the steps (2) and (3) are as follows: selecting anion analysis chromatographic column with column temperature of 25-40 deg.C; the flow rate is 0.5-5 mL/min; the leacheate is potassium hydroxide solution.
Preferably, the livestock meat in the step (1) is selected from pork, beef, mutton, chicken or duck.
Preferably, the temperature of ultrasonic extraction in the step (1) is 30-50 ℃; more preferably, the temperature is 40 ℃.
Preferably, the ultrasonic extraction time in the step (1) is 20-40 min; more preferably, the ultrasonic extraction time is 30 min.
Preferably, the heating temperature of the water bath in the step (1) is 60-80 ℃; more preferably, the water bath heating temperature is 75 ℃.
Preferably, the heating time of the water bath in the step (1) is 2-10 min; more preferably, the heating time in the water bath is 5 min.
Preferably, the organic solvent in step (1) is selected from dichloromethane, acetone, acetonitrile or a combination thereof.
More preferably, the organic solvent is dichloromethane.
Preferably, the mass-to-volume ratio of the homogeneous sample to the organic solvent in the step (1) is 1 g: 1-10mL, more preferably 1 g: 5 mL.
Preferably, the quantitative limits of nitrate and nitrite in step (2) are 0.3mg/kg and 0.2mg/kg respectively, and the detection limits are 0.09mg/kg and 0.06mg/kg respectively.
Preferably, the nitrate nitrogen in the step (2) has a good linear relation in the range of 0.2-2.0 mg/kg.
Preferably, the nitrite in the step (2) is in a good linear relationship in the range of 0.02-0.2 mg/kg.
Preferably, the anion analysis chromatographic column in the steps (2) and (3) is a Dionex IonPacTMAS11-HCRFICTMAn Analytical type ion chromatography column.
Preferably, the column temperature in steps (2) and (3) is 30 ℃.
Preferably, the flow rate of the rinsing liquid in the steps (2) and (3) is 1 mL/min.
Preferably, the elution gradient of the potassium hydroxide leacheate in the steps (2) and (3) is ① 5mmol/L for 40-50min, ② 60mmol/L for 5-15min, and ③ 5mmol/L for 5-15 min.
Preferably, the elution gradient of the potassium hydroxide eluent in the steps (2) and (3) is ① 5mmol/L for 45-50min, ② 60mmol/L for 10min, and ③ 5mmol/L for 10 min.
More preferably, the elution gradient of the potassium hydroxide eluate in the steps (2) and (3) is as follows:
the invention has the positive and beneficial effects that:
by optimizing the pretreatment method and the instrument detection conditions, the detection method disclosed by the invention makes up for the defects of detection by a national standard method, has the advantages of simplicity in operation, short test period, low loss, high recovery rate, good precision and the like, can effectively reduce the interference of impurities on the detection of nitrate and nitrite, and is suitable for rapid determination of nitrate and nitrite in meat and meat products.
Detailed Description
The present invention will be further described with reference to the following examples, but the embodiments of the present invention are not limited thereto. The experimental procedures used in the following examples are all conventional procedures unless otherwise specified.
Test example 1 detection of nitrate and nitrite contents in livestock and poultry meat by the method of the present invention
1. Test materials and reagents
(1) Test materials: the tested materials include various livestock and poultry meat and products thereof, such as pork, beef, mutton, chicken, duck meat, cured meat products, jerky products, western meat products and other samples, which are purchased from Nanjing farmer markets and supermarkets.
(2) Reagent: nitrate standard solution and nitrite standard solution (both 200 mg/kg)-1In terms of concentration of each nitrate ion), all purchased from beijing coast hongmeng standard substance technology llc; methylene chloride (analytically pure), methanol (analytically pure), and potassium hydroxide (analytically pure) were purchased from national pharmaceutical group chemical agents, ltd. All solutions were prepared with ultrapure deionized water.
2. Apparatus and device
Ion chromatographs (model ICS5000, equipped with a conductivity detector, AERS type suppressor, CR-TC trap column), RP columns and Na columns, all available from Thermo Fisher, usa; high speed refrigerated centrifuge (D-16C), analytical balance (CPA224S), all available from Sartorius, Germany; a water bath (TW20) available from JULABO, Germany; ultrasonic cleaner (X025-12DTD) available from Nanjing pioneer Europe instruments Inc.; various range micropipettes are available from Eppendorf, germany.
3. Experimental methods
(1) Sample pretreatment
The method comprises the following steps: weighing 2g of homogeneous sample (accurate to 0.0001g), placing in a 50mL centrifuge tube, adding 30mL of ultrapure water, performing ultrasonic extraction at 40 ℃ for 30min, and shaking for 1 time every 5 min; heating in 75 deg.C water bath for 5min, taking out, cooling to room temperature, adding 10mL dichloromethane, shaking, layering, standing，5000r·min-1Centrifuging for 10 min; taking the supernatant, sequentially passing through a 0.22 mu m filter membrane, an RP column and a Na column, discarding the first 3mL of supernatant, and waiting for detection on a machine. Except for the non-weighed sample, the corresponding blank control experiment is completed at the same time according to the operation.
The national standard method comprises the following steps: the pretreatment method was carried out according to the first method of the national food safety Standard for the determination of nitrite and nitrate in food (GB 5009.33-2016).
(2) Filter column and filter membrane activation
The filter column and the filter membrane are required to be activated before being used for extraction, and the activation process comprises the following steps: sequentially passing through an RP column by using 5mL of methanol and 10mL of ultrapure water, standing and activating for 30 min; the 0.22 μm filter was passed through 10mL of ultrapure water, and left to stand for 30min for activation.
(3) Establishment of chromatographic conditions
A chromatographic column: using Dionex IonPacTMAS11-HC RFICTMAnalytical type ion chromatography column (4 mm. times.250 mm) equipped with Dionex IonPacTMAG11-HC RFICTMGuard type Guard column (4 mm. times.50 mm).
The detection conditions are as follows: column temperature, 30 ℃; suppressor current, 149 mA; flow Rate, 1.0 mL. min-1(ii) a Sample size, 100 μ L; potassium hydroxide leacheate, the leaching conditions of which are shown in table 1.
TABLE 1 gradient elution conditions
(4) Standard curve making and detection limit and quantitative limit determination
According to the optimum detection conditions determined by the tests, nitrate and nitrite are prepared into a series of mixed standard working solutions with the concentration of nitrate ions of 0.2, 0.4, 0.6, 0.8, 1.0, 1.5 and 2.0mg/kg and the concentration of nitrite ions of 0.02, 0.04, 0.06, 0.08, 0.1, 0.15 and 0.2mg/kg, and the mixed standard working solutions are tested on a computer. And (3) drawing a standard curve by taking the mass concentration (mg/kg) of the nitrate ions and the nitrite ions as an abscissa (X) and taking the peak area (mu S multiplied by min) as an ordinate (Y), so as to determine the optimal linear range and the correlation coefficient. The limit of detection (LOD) is calculated by 3 times the signal-to-noise ratio, and the limit of quantification (LOQ) is calculated by 10 times the signal-to-noise ratio.
(5) Precision and recovery from spiked samples
The method comprises the steps of mincing meat of five livestock and poultry such as pigs, cattle, sheep, chickens and ducks, and respectively adding mixed standard solutions of nitrate and nitrite with low, medium and high concentration levels. The sample was pretreated as described above, and the sample was repeatedly introduced 6 times into a standard sample of the same concentration, and the recovery and precision (RSD) of the sample was calculated.
4. Data analysis
Data were analyzed using Chromeleon Client Program Software from Thermo Fisher Scientific, USA, and charted using Microcal Origin 7.5(Microcal Software, Inc.) Software. Performing parallel measurement 6 times in a standard addition recovery experiment, and calculating the RSD; the samples were run in duplicate 3 times and the average was calculated.
5. Test results and analysis
(1) Detection limit, quantitative limit and linear range
The ion chromatograms of nitrate and nitrite show that the retention time of nitrite and nitrate are 16.040min and 35.633min, respectively, the peak time difference between them is large, and the separation degree is good.
Nitrate and nitrite standard curves are plotted to determine the quantitative, detection and linear limits for nitrate and nitrite. As is clear from Table 2, the quantitative limits of nitrate and nitrite were 0.3 and 0.2mg/kg, respectively, and the detection limits were 0.09 and 0.06mg/kg, respectively. The nitrate is 0.2-2.0mg/kg, the nitrite is in good linear relation in the range of 0.02-0.2mg/kg, and the correlation coefficients are all 0.999.
TABLE 2 Linear equation, Linear coefficient, quantitation limit and detection limit for nitrate and nitrite
(2) Recovery and precision of the added standard
Because the background values of the nitrate and the nitrite in the livestock meat detected by the detection method and the national standard method are different, the additive amount of the nitrate and the nitrite is respectively calculated according to the background values of the samples in the test. The results of the detection of the recovery rates of 5 meat of livestock and poultry of pig, cattle, sheep, chicken and duck are shown in tables 3 and 4, and the average value of the normalized recovery rates of nitrate and nitrite measured by the detection method of the invention is 77.0-106.1%, 77.3-101.0%, 65-97.5%, 80.0-103.3% and 90.5-99.2% respectively at low, medium and high concentration levels, and the RSD is 1.12-8.75%, 2.48-7.05%, 1.34-6.83%, 1.29-7.70% and 0.10-8.20% respectively. The average value of the standard recovery rates of nitrate and nitrite measured by the national standard method is respectively 30.8-76.8%, 16.7-83.0%, 51.7-89.2%, 25.4-63.0% and 50.3-80.0%, and the RSD is respectively 1.82-10.40%, 1.02-12.26%, 2.41-13.34%, 1.14-11.49% and 2.36-13.01%. This shows that compared with the national standard method, the detection method of the invention has higher recovery rate and good precision.
Table 3 recovery of the process of the invention with addition of standard and RSD (n ═ 6)
Table 4 national standard methods standard recovery and RSD (n ═ 6)
Test example 2 practical application of the detection method of the present invention
Selecting 14 parts of commercial livestock and poultry meat products, wherein 4 parts of cured meat products, 3 parts of sauced marinated products, 3 parts of jerky products, 1 part of barbecue products and 3 parts of western-style meat products, and detecting the contents of nitrate and nitrite in the meat products. The sample pretreatment method and the detection conditions refer to test example 1, so that the practical application effect of the method for detecting the contents of nitrate and nitrite in the livestock and poultry meat products is evaluated.
As shown in Table 5, the selected commercial meat products all contained certain amounts of nitrate and nitrite. The nitrate content is 1.4270-37.0629mg/kg, wherein the content of the pork jerky is higher than the national maximum residual quantity (30 mg/kg). In addition, the nitrate content in the sauced beef, the dried meat floss and the roast duck is detected, but the nitrate content does not exceed the standard. The nitrite content is 0.0468-10.6934mg/kg, wherein the content of the starch-free ham is the highest, but is lower than the national limit maximum residue (30 mg/kg).
TABLE 5 nitrate and nitrite content in livestock and poultry meat products
Claims (10)
1. A method for detecting nitrate and nitrite in livestock meat and products thereof is characterized by comprising the following steps:
(1) sample pretreatment: weighing a homogeneous sample of livestock and poultry meat, adding water for ultrasonic extraction, heating in a water bath, taking out, cooling to room temperature, adding an organic solvent, fully mixing, standing, centrifuging, and taking supernatant to sequentially pass through a 0.22 mu m filter membrane, an RP column and a Na column for later use;
(2) and (3) preparing a standard curve: respectively injecting the standard series working solution of nitrate ions and nitrite ions into an ion chromatograph to obtain standard working solution chromatograms with various concentrations, measuring corresponding peak areas, and drawing standard curves of the nitrate ions and the nitrite ions by taking the mass concentrations of the nitrate ions and the nitrite ions as horizontal coordinates and the peak areas as vertical coordinates;
(3) and (3) content determination of the solution to be detected: injecting the blank solution and the solution to be detected into an ion chromatograph to obtain peak areas of the blank solution and the sample solution, and calculating the content of nitrate and nitrite in the solution to be detected according to a standard curve;
wherein, the ion chromatography conditions in the steps (2) and (3) are as follows: selecting anion analysis chromatographic column with column temperature of 25-40 deg.C; the flow rate is 0.5-5 mL/min; the leacheate is potassium hydroxide solution.
2. The detection method according to claim 1, wherein the livestock meat in the step (1) is pork, beef, mutton, chicken or duck.
3. The detection method according to claim 1, wherein the temperature of the ultrasonic extraction in the step (1) is 30-50 ℃, and the time of the ultrasonic extraction is 20-40 min.
4. The detection method according to claim 1, wherein the heating temperature of the water bath in the step (1) is 60-80 ℃, and the heating time of the water bath is 2-10 min.
5. The detection method according to claim 1, wherein the organic solvent in step (1) is selected from dichloromethane, acetone, acetonitrile, or a combination thereof.
6. The detection method according to claim 1, wherein the mass-to-volume ratio of the homogeneous sample to the organic solvent in the step (1) is 1 g: 1-10 mL.
7. The detection method according to claim 1, wherein the column temperature in the steps (2) and (3) is 30 ℃.
8. The detection method according to claim 1, wherein the flow rate of the rinsing solution in the steps (2) and (3) is 1 mL/min.
9. The detection method as claimed in claim 1, wherein the anion analysis chromatographic column in the steps (2) and (3) is a Dionex IonPacTMAS11-HC RFICTMAn Analytical type ion chromatography column.
10. The detection method according to claim 1, wherein the elution gradient of the potassium hydroxide eluate in the steps (2) and (3) is ① 5mmol/L for 40-50min, ② 60mmol/L for 5-15min, ③ 5mmol/L for 5-15 min.
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| CN113804795A (en) * | 2021-10-08 | 2021-12-17 | 河南润弘制药股份有限公司 | Method for detecting nitrate impurities in nitroglycerin solution and injection |
| CN115128188A (en) * | 2022-07-11 | 2022-09-30 | 天津力生制药股份有限公司 | Detection method for nitrite in metronidazole and metronidazole tablets |
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| CN115128188A (en) * | 2022-07-11 | 2022-09-30 | 天津力生制药股份有限公司 | Detection method for nitrite in metronidazole and metronidazole tablets |
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