CN106501403B - A method of it is used for while detecting sodium propionate (calcium) and sodium Diacetate - Google Patents
A method of it is used for while detecting sodium propionate (calcium) and sodium Diacetate Download PDFInfo
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
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Abstract
The invention discloses a kind of methods for being used for while detecting sodium propionate (calcium) and sodium Diacetate.Sample treatment: sample to be tested is accurately weighed in kjeldahl determination distilling apparatus, the phosphoric acid solution of 1mL1mol/L is added, carry out steam distillation, distillate is after condensation, use colorimetric cylinder as reception device, it is to be distilled go out 23.5-24.5mL distillate when stop receiving, adjust pH value to 2.7-3.5, add water to be settled to 25ml, shakes up；It refilters to obtain filtrate；Above-mentioned gained is subjected to HPLC detection；The mass concentration of sodium Diacetate in sample is calculated according to the linear equation of propionic acid and sodium Diacetate.This method has greatly saved the sample process time, and matrix interference is few, easy to operate；The linear relationship of method is good, the rate of recovery is high, quantitative limit is low, reproducible；It is practical, can simultaneously suitable for the food such as oyster sauce, soy sauce and fish sauce sodium propionate (calcium) and sodium Diacetate content measurement.
Description
Technical field
The present invention relates to field of food detection, more particularly to a kind of it is used for while detecting sodium propionate (calcium) and sodium Diacetate
Method.
Background technique
Application of the use of food additives in processed food and instant food is more and more extensive.Processed food,
If oyster sauce, soy sauce, fish sauce add preservative in the production process to inhibit microorganism to generate, nutritive value and other spies are maintained
Property, and then extend effective period of food quality.However, illegally adding and preservative, which is excessively added, can make consumer have allergic reaction and chronic
Poisoning risk.Therefore, " national food safety standard food additives use standard " (GB 2760-2014) defines all anti-
The maximum allowable addition concentration of rotten agent.
Oyster sauce, soy sauce, fish sauce are the flavouring being favourably welcome on people's dining table.Sodium propionate (calcium), sodium Diacetate conductization
Preservative is learned, is widely used in the food such as cake, soy sauce.It is provided in GB 2760-2014, propionic acid and its sodium salt, calcium salt
Maximum allowable usage amount in soy sauce is 2.5g/kg, and must not be used in oyster sauce, fish sauce；Sodium Diacetate oyster sauce, soy sauce and
Maximum usage amount in fish sauce is 2.5g/kg.The detection method of propionic acid has gas chromatography and high performance liquid chromatography in food
Method etc..The detection method high performance liquid chromatography of sodium Diacetate and the chromatography of ions etc..Woods Qinghe etc., Wuzhong be emerging etc. and Xiang Linmin
Etc. the method for reporting high performance liquid chromatography while measuring (calcium) and sodium Diacetate of sodium propionate in cake.Xiang Wenjuan etc. is reported entirely
Sodium propionate (calcium) and sodium Diacetate in automatic Solid Phase Extraction (SPE)-HPLC method measurement food.Zhu Hongliang etc. reports efficient liquid
The method that phase chromatography measures (calcium) and sodium Diacetate of sodium propionate in food simultaneously.Li Min etc. reports high performance liquid chromatography simultaneously
Measure sodium Diacetate and propionic acid calcium content in Cangshan garlic rice.On September 29th, 2014, China have received the Xiamen enterprise of South Korea's notification
Industry oyster sauce detects the unqualified food information of propionic acid, and China national food safety standard GB2760 must not also make in regulation oyster sauce
With propionic acid, but there is not been reported in relation to the detection method of sodium propionate (calcium) and sodium Diacetate content in the food such as oyster sauce.
Related sodium propionate in GB/T 5009.120-2003, GB/T 23382-2009 and GB/T 23383-2009
The way of distillation of (calcium) and sodium Diacetate content detection is to weigh 25g sample in 500mL cucurbit, distillation to 250mL capacity
In bottle, final constant volume is 250mL.The detection method needs sample size big, and constant volume is larger, and more time-consuming.
Summary of the invention
Quick, easy, accurate, practical it can be used to detect sodium propionate (calcium) simultaneously the purpose of the present invention is to provide a kind of
With the method for sodium Diacetate.
To achieve the above object, the present invention provides a kind of method for being used for while detecting sodium propionate (calcium) and sodium Diacetate,
It is characterized by comprising the following steps
Sample treatment: accurately weighing sample to be tested in kjeldahl determination distilling apparatus, and 1~3mL0.5~3mol/L is added
Phosphoric acid solution carries out steam distillation, and distillate uses colorimetric cylinder as reception device, 23.5- out to be distilled after condensation
Stop receiving when 24.5mL distillate, with the pH value of the phosphoric acid solution tune distillate of 0.5~3mol/L to 2.7-3.5, adds water fixed
Hold to 25ml, shakes up；Filtered solution is obtained through 0.22~0.45 μm of filtering with microporous membrane again；The pH value for adjusting distillate is 2.7-
3.5, in this pH value range, sodium propionate (calcium) and sodium Diacetate can be fully converted to propionic acid and acetic acid is detected；
HPLC: above-mentioned gained filtered solution is subjected to HPLC；
Detection method: according to the linear equation y1=284.58x1+0.210 of propionic acid, wherein x1 is the mass concentration of propionic acid,
Y1 is the peak area of propionic acid；The mass concentration of propionic acid in sample can be calculated；
According to the linear equation y2=236.24x2+0.298 of sodium Diacetate, wherein x2 is the mass concentration of sodium Diacetate,
Y2 is the peak area of sodium Diacetate；The mass concentration of sodium Diacetate in sample can be calculated.
Further, in the sample treatment, sample to be tested 5.00g is accurately weighed in kjeldahl determination distilling apparatus.
Further, the condition of the HPLC is chromatographic column: C18 column, 250mm × 4.6mm × 5 μm or equivalent chromatographic column；Column
Temperature: 20~40 DEG C；Mobile phase is 1.5g/L ammonium dihydrogen phosphate, and solvent is the mixed liquor of first alcohol and water, with 0.5~3mol/L
Phosphoric acid solution adjusts pH to 2.7~3.5；Flow velocity: 0.5~2mL/min；Sample volume: 10~20 μ L.
Further, in the HPLC step, solvent is the mixed liquor of the first alcohol and water of volume ratio 5:95~10:90.
Further, in the HPLC step, solvent is the mixed liquor of the first alcohol and water of volume ratio 10:90.
Further, the sample to be tested is oyster sauce, soy sauce or fish sauce.
The present invention refers to national regulations method, using oyster sauce, soy sauce and fish sauce as matrix, for the first time using kjeldahl determination distillation dress
It sets, using high-efficient liquid phase chromatogram technology, establishes and can detect oyster sauce simultaneously, sodium propionate (calcium) and sodium Diacetate in soy sauce and fish sauce
Method, need to be only 5g with sample size, constant volume is that (sample size greatly reduces 25mL, and constant volume also greatly reduces.Because
It is steam distillation, constant volume reduction means to save energy and time).This method is for the first time in sodium propionate (calcium) and diacetic acid
Kjeldahl determination distilling apparatus is used in sodium content detection, it is quick, easy, accurate, practical.
Oyster sauce is a kind of flavouring of unique flavor, it has natural marine product flavor, delicious strong flavour, and
It is easy to use, it is full of nutrition, rich in microelements such as Ca, Fe, Zn, Se.Soy sauce is one of common flavouring in people's life,
And it also has anti-oxidant equal nutrition health-care functions other than seasoning acts on.Fish sauce rich in a variety of amino acid and Cu, Cr,
The microelements such as Zn, I not only have unique sea food flavor, there are also anti-oxidant, blood pressure lowering, reduce the functional characteristics such as cholesterol.Oyster
Oil, soy sauce, fish sauce are all the flavouring being favourably welcome on people's dining table, and wherein the detection and monitoring of food additives content are
The important channel to ensure food safety.The present invention combines kjeldahl determination distilling apparatus for the first time, and oyster sauce, sauce can be detected simultaneously by establishing
The high performance liquid chromatography of sodium propionate (calcium) and sodium Diacetate content in oil and fish sauce.
This research is using oyster sauce, soy sauce and fish sauce as matrix, with reference to national regulations method, and combines this laboratory to analysis side
The verifying experience of method, methodology validation index include the determination of mobile phase, the determination of object distillation volume, linear equation, determine
Amount limit, accuracy and precision.The present invention compares different mobile phases, finally selectes methanol-water (10/90, v/v) as molten
Agent mobile phase, sodium Diacetate and sodium propionate appearance time are respectively 4.91 and 10.18min, and baseline is steady, peak type and appearance time
Stablize；Meanwhile four kinds of distillate volumes are compared, it is final to determine that distillate volume is 25mL, sodium propionate (calcium) and sodium Diacetate
The rate of recovery can respectively reach 100.3% and 98.2%.The detection of this method is limited to 0.010g/kg, is quantitatively limited to 0.025g/
kg；In three kinds of matrix, the rate of recovery of sodium propionate (calcium) (in terms of propionic acid) and sodium Diacetate is respectively 88.5%~108.3% He
86.5%~108.7%, relative standard deviation is 2.13%~6.42% and 2.02%~6.37%, is able to satisfy sodium propionate
The detection of (calcium) and sodium Diacetate needs.
In conclusion this method has greatly saved the sample process time, matrix interference is few, easy to operate；Method it is linear
Relationship is good, the rate of recovery is high, quantitative limit is low, reproducible；It is practical, the food such as oyster sauce, soy sauce and fish sauce can be suitable for simultaneously
The measurement of sodium propionate (calcium) and sodium Diacetate content in product.
Detailed description of the invention
Fig. 1 is propionic acid and sodium Diacetate standard chromatogram in embodiment 2.
Fig. 2 is propionic acid in embodiment 3, sodium Diacetate distillate volume and rate of recovery figure.
Specific embodiment
The embodiment of the present invention is described below in detail, examples of the embodiments are shown in the accompanying drawings, wherein from beginning to end
Same or similar label indicates same or similar element or element with the same or similar functions.Below with reference to attached
The embodiment of figure description is exemplary, it is intended to is used to explain the present invention, and is not considered as limiting the invention.Embodiment
In particular technique or condition person is not specified, described technology or conditions or according to the description of product according to the literature in the art
Book carries out.Reagents or instruments used without specified manufacturer, being can be with conventional products that are commercially available.
Following embodiment instrument: 1260 liquid chromatograph of Agilent is furnished with DAD detector；German Sai Duolisi
Electronic balance, sensibility reciprocal 0.1mg and 0.01g；Kjeldahl determination distilling apparatus.
Sodium propionate in following embodiment can be substituted by calcium propionate.
Method:
Sample treatment: accurately weighing sample in kjeldahl determination distilling apparatus, and the phosphoric acid solution of 1mL 1mol/L is added, into
Row steam distillation, distillate use 25mL colorimetric cylinder as reception device after condensation, it is to be distilled go out about 24mL when stopping connect
It receives, with phosphoric acid solution tune pH value of 1mol/L to 2.7-3.5 or so, adds water to be settled to 25ml, shake up.Through 0.22 μm of miillpore filter
After filtering, measured for HPLC.
HPLC: chromatographic column: Sapphire C18 (250mm × 4.6mm × 5 μm), column temperature: 30 DEG C；Mobile phase is 1.5g/L
Ammonium dihydrogen phosphate (mixed liquor that solvent is methanol-water), adjusts pH to 2.7~3.5 with 1mol/L phosphoric acid solution；Flow velocity:
1mL/min；Sample volume: 10 μ L.
Embodiment 1: standard mixed solution is prepared
The preparation of sodium propionate standard reserving solution: 1.3g (being accurate to 0.0001g) sodium propionate is accurately weighed, is settled to water
100mL is configured to be equivalent to the sodium propionate standard reserving solution of the propionic acid containing 10mg/mL.
The preparation of sodium Diacetate standard reserving solution: 1.0g (being accurate to 0.0001g) sodium Diacetate is accurately weighed, with water constant volume
To 100mL, it is configured to the sodium Diacetate standard reserving solution of 10mg/mL.
Successively draw 0.0125,0.05,0.125,0.5,1.25,2.5mL sodium propionate and sodium Diacetate standard reserving solution in
The phosphoric acid solution 1mL of 1mol/L is added in kjeldahl determination distilling apparatus, when distilling out about 24mL, with the phosphoric acid solution tune of 1mol/L
PH value is settled to 25mL to 3 or so.Obtain sodium propionate (being equivalent to propionic acid), the hybrid working liquid concentration of sodium Diacetate is respectively
0.005,0.02,0.05,0.2,0.5,1.0mg/mL.By 0.22 μm of filtering with microporous membrane, concentration sample introduction from low to high, with dense
Degree is abscissa, peak area is ordinate, draws standard curve.Obtain: the linear equation of propionic acid is y=284.58x+0.210,
The linear equation of sodium Diacetate is y=236.24x+0.298.The linearly dependent coefficient of linear equation is 0.9999.
Embodiment 2: the determination of mobile phase
HPLC condition:
Chromatographic column: Sapphire C18 (250mm × 4.6mm × 5 μm), column temperature: 30 DEG C；Mobile phase is 1.5g/L di(2-ethylhexyl)phosphate
Hydrogen ammonium salt solution (solvent is following three kinds of solvents), adjusts pH to 2.7~3.5 with 1mol/L phosphoric acid solution；Flow velocity: 1mL/min；Into
Sample amount: 10 μ L.Three kinds of solvents are: water, methanol-water (10/90, v/v), methanol-water (15/85, v/v).
1.5g diammonium hydrogen phosphate is weighed respectively in the above-mentioned three kinds of solvents of 1L, is adjusted to pH value extremely with 1mol/L phosphoric acid solution
2.7~3.5.Propionic acid and sodium Diacetate are separated with these three mobile phases respectively.
Test result shows: mobile phase is done using pure water, larger to the injury of chromatographic column, the appearance time of propionic acid is later,
And peak is wider.It is used as mobile phase using methanol-water (15/85, v/v), the peak appearance time of sodium Diacetate is too early, dry by matrix
Disturb it is larger, and due to select 214nm wavelength be used as Detection wavelength, organic Phase Proportion it is excessively high after baseline injustice.Use methanol-water
The mobile phase of (10/90, v/v) as solvent, as a result as shown in Figure 1, sodium Diacetate and sodium propionate appearance time are respectively 4.91
And 10.18min.Baseline is steady, and peak type and appearance time are stablized.
Embodiment 3: the determination of object distillate volume
Commercially available oyster sauce blank sample 5.00g is taken, wherein the concentration of propionic acid and sodium Diacetate mark-on is 1.0g/kg, blank
Sodium propionate (calcium) and sodium Diacetate in sample, it is acidified to be converted to propionic acid and acetic acid, using steam distillation, condensation
After pipe is cooling, distillate is received with colorimetric cylinder.Distillate volume is optimized in this experiment: each distillation volume parallel 6
Group test, is shown in Fig. 2.As shown in Figure 2, the rate of recovery of propionic acid and sodium Diacetate increases with the increase of distillate volume, distillates
Liquid product be 10mL when, the average recovery rate of sodium propionate (calcium) and sodium Diacetate only have 50.2% (RSD=3.2%, n=6) and
52.1% (RSD=4.3%, n=6)；When distillate volume is 15mL, the average recovery rate of sodium propionate (calcium) and sodium Diacetate is only
There are 74.3% (RSD=2.5%, n=6) and 71.9% (RSD=4.1%, n=6)；When distillate volume is 20mL, sodium propionate
The average recovery rate of (calcium) and sodium Diacetate is 92.1% (RSD=4.1%, n=6) and 94.5% (RSD=3.1%, n=6)；
When distillate volume reaches 25mL, the rate of recovery of sodium propionate (calcium) and sodium Diacetate is averagely respectively 100.3% (RSD=
2.0%, n=6) and 98.2% (RSD=2.5%, n=6).Therefore, it is final constant volume that selection distillation volume, which is 25mL,.
Embodiment 4: the equation of linear regression and quantitative limit of method
Take sodium propionate (calcium) (in terms of propionic acid), sodium Diacetate mass concentration 0.005,0.02,0.05,0.2,0.5,1.0mg/
6 mixed standard solutions of mL, according to concentration successively sample introduction from low to high, using respective mass concentration as abscissa (g/mL),
Peak area is ordinate, obtains equation of linear regression, and the linear equation of propionic acid is y=284.58x+0.210, the line of sodium Diacetate
Property equation be y=236.24x+0.298.The linearly dependent coefficient of linear equation is 0.9999, and sodium propionate (calcium) is (with propionic acid
Meter), sodium Diacetate good linear relationship is presented in the range of linearity of 0.005~1.000mg/mL.With 3 times of signal-to-noise ratio (S/N
=3) corresponding target concentration is detection limit, using the corresponding target concentration of 10 times of signal-to-noise ratio (S/N=10) as quantitative limit,
The instrument detection limit for obtaining two kinds of substances is 0.002mg/mL, and instrument quantitative limit is 0.005mg/mL.The detection limit of instrument
And quantitative limit, multiplied by constant volume (25mL), divided by sample quality (5.00g), the possibility detection for obtaining method is limited to
0.010g/kg may quantitatively be limited to 0.025g/kg.Negative sample (not containing the sample of sodium propionate and sodium Diacetate) is taken, is added
Enter sodium propionate and sodium Diacetate, makes the concentration 0.010g/kg of sodium propionate in sample (in terms of propionic acid) and sodium Diacetate, according to reality
Proved recipe method handles sample, and the signal-to-noise ratio for measuring object signal is greater than 3.Take negative sample (i.e. without containing sodium propionate and diacetic acid
The sample of sodium), sodium propionate and sodium Diacetate is added, makes the concentration of (in terms of the propionic acid) and sodium Diacetate of sodium propionate in sample
0.025g/kg handles sample according to 1.4 experimental methods, and the signal-to-noise ratio for measuring object signal is greater than 10.So that it is determined that method
Detection is limited to 0.010g/kg, is quantitatively limited to 0.025g/kg.
This experiment method for building up and national standard method (GB/T 23382-2009 and GB/T 23383-2009) are compared such as 1 institute of table
Show.This experiment method for building up, can detect two projects of propionic acid and sodium Diacetate simultaneously, and GB/T 23382-2009 and GB/T
23383-2009 only individually detects propionic acid and sodium Diacetate project.It is only 5.00g that this detection method, which needs sample size, most
Whole constant volume is 25mL, and compared with national standard detection method, required sample size is reduced and constant volume reduces；Meanwhile single sample
The product vapor consuming time, which also foreshortens to, only needs 10min.The rate of recovery of this detection method can be consistent with national standard method, be existed
86.5% or more；In terms of method quantitative limit, propionic acid is accurate to 0.025g/kg by 0.10g/kg, and sodium Diacetate is by 0.05g/kg essence
Really to 0.025g/kg.
1 experiment method for building up of table and national standard method deck watch
Embodiment 5: the accuracy and precision of method
Recovery test is added to oyster sauce, soy sauce and fish sauce etc. respectively, wherein oyster sauce is positive sample, the detection of propionic acid
Amount is 0.132g/kg, remaining two kinds are negative sample.Mark-on is carried out according to the distillating method of the chromatographic condition of optimization, this method
Recovery test.Spiked levels choose 3 concentration: minimum concentration chooses quantitative limit concentration 0.030g/kg nearby；Second concentration choosing
Take maximum allowable usage amount concentration 2.5g/kg；Third concentration is that (distillation after constant volume is molten by range of linearity extracellular concentration 6.0g/kg
Liquid is detected after diluting one times with instrument).Weigh 3 parts of 100g sample, be separately added into 3.9mg sodium propionate and 3.0mg sodium Diacetate,
324.3mg sodium propionate and 250.0mg sodium Diacetate and 778.4mg sodium propionate and 600.0mg sodium Diacetate sufficiently dissolve, make
The spiked levels of propionic acid and sodium Diacetate are 0.030g/kg, 2.5g/kg and 6.0g/kg in sample.Mark-on examination is accurately weighed respectively
Sample 5.00g (being accurate to 0.01g) is handled according to 1.4 experimental methods and is measured in kjeldahl determination distilling apparatus, and each concentration repeats
Six parallel laboratory tests, accuracy and precision the results are shown in Table 2.As shown in Table 2, in three kinds of matrix, sodium propionate (calcium) is (with propionic acid
Meter) and the rate of recovery of sodium Diacetate be respectively 88.5%~108.3% and 86.5%~108.7%, relative standard deviation is
2.13%~6.42% and 2.02%~6.37%.The rate of recovery of this method is high, and precision is good, can satisfy sodium propionate (calcium) and
The detection of sodium Diacetate needs.
2 sodium propionate of table (calcium) (in terms of propionic acid), the sodium Diacetate rate of recovery and relative standard deviation (RSD) (n=6) table
Although the embodiments of the present invention has been shown and described above, it is to be understood that above-described embodiment is example
Property, it is not considered as limiting the invention, those skilled in the art are not departing from the principle of the present invention and objective
In the case where can make changes, modifications, alterations, and variations to the above described embodiments within the scope of the invention.
Claims (5)
1. a kind of method for detecting sodium propionate or calcium propionate and sodium Diacetate simultaneously, which is characterized in that include the following steps,
Sample treatment: accurately weighing sample to be tested in kjeldahl determination distilling apparatus, and 1~3mL0.5~3mol/L phosphoric acid is added
Solution carries out steam distillation, and distillate uses colorimetric cylinder as reception device, 23.5-24.5mL out to be distilled after condensation
Stop receiving when distillate, with the pH value of the phosphoric acid solution tune distillate of 0.5~3mol/L to 2.7-3.5, water is added to be settled to
25ml shakes up；Filtrate is obtained through 0.22~0.45 μm of filtering with microporous membrane again；
HPLC detection: above-mentioned gained filtrate is subjected to HPLC detection；The condition of the HPLC is chromatographic column: C18 column, 250mm ×
4.6mm×5μm；Column temperature: 20~40 DEG C；Mobile phase is 1.5g/L ammonium dihydrogen phosphate, and solvent is the mixed liquor of first alcohol and water,
PH to 2.7~3.5 is adjusted with 0.5~3mol/L phosphoric acid solution；Flow velocity: 0.5~2mL/min；Sample volume: 10~20 μ L；
Detection method: according to the linear equation y1=284.58x1+0.210 of propionic acid, wherein x1 is the mass concentration of propionic acid, and y1 is
The peak area of propionic acid；The mass concentration of propionic acid in sample can be calculated；
According to the linear equation y2=236.24x2+0.298 of sodium Diacetate, wherein x2 is the mass concentration of sodium Diacetate, and y2 is
The peak area of sodium Diacetate；The mass concentration of sodium Diacetate in sample can be calculated.
2. the method for being used for described in claim 1 while detecting sodium propionate or calcium propionate and sodium Diacetate, which is characterized in that described
In sample treatment, sample to be tested 5.00g is accurately weighed in kjeldahl determination distilling apparatus.
3. the method for being used for described in claim 1 while detecting sodium propionate or calcium propionate and sodium Diacetate, which is characterized in that described
In HPLC step, solvent is the mixed liquor of the first alcohol and water of volume ratio 5:95~10:90.
4. the method for being used for described in claim 1 while detecting sodium propionate or calcium propionate and sodium Diacetate, which is characterized in that described
In HPLC step, solvent is the mixed liquor of the first alcohol and water of volume ratio 10:90.
5. the method for being used for described in claim 1 while detecting sodium propionate or calcium propionate and sodium Diacetate, which is characterized in that described
Sample to be tested is oyster sauce, soy sauce or fish sauce.
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| CN109406710A (en) * | 2018-11-26 | 2019-03-01 | 谱尼测试集团股份有限公司 | A kind of liquid-phase chromatography method detecting sodium Diacetate |
| CN109813822A (en) * | 2019-02-14 | 2019-05-28 | 上海爱普食品工业有限公司 | The detection method of propionic acid content in acid hydrolyzed vegetable protein |
| CN109900652B (en) * | 2019-04-29 | 2021-06-04 | 北京普赞生物技术有限公司 | Rapid detection method for sodium diacetate in food |
| CN110208415A (en) * | 2019-06-24 | 2019-09-06 | 河南省口岸食品检验检测所 | The detection method of sodium Diacetate in a kind of flour |
| CN112763629A (en) * | 2021-01-18 | 2021-05-07 | 上海美农生物科技股份有限公司 | Method for simultaneously detecting 6 acidifiers in compound acidifier |
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| 高效液相色谱法测定食品中双乙酸钠和丙酸盐含量;朱洪亮;《食品安全质量检测学报》;20140731;第5卷(第7期);全文 |
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