CN111965314A - Infant formula milk powder based chlorate and perchlorate standard sample and preparation method thereof - Google Patents
Infant formula milk powder based chlorate and perchlorate standard sample and preparation method thereof Download PDFInfo
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- CN111965314A CN111965314A CN202010817037.9A CN202010817037A CN111965314A CN 111965314 A CN111965314 A CN 111965314A CN 202010817037 A CN202010817037 A CN 202010817037A CN 111965314 A CN111965314 A CN 111965314A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/02—Food
- G01N33/04—Dairy products
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N1/00—Sampling; Preparing specimens for investigation
- G01N1/28—Preparing specimens for investigation including physical details of (bio-)chemical methods covered elsewhere, e.g. G01N33/50, C12Q
- G01N1/44—Sample treatment involving radiation, e.g. heat
Abstract
The invention discloses a preparation method of a standard sample of infant formula milk powder chlorate and perchlorate, which comprises the following steps: accurately weighing high-purity sodium chlorate and high-purity sodium perchlorate, and adding the high-purity sodium chlorate and high-purity sodium perchlorate into primary water to prepare chlorate and perchlorate solution; step two, quantitatively weighing the matrix emulsion powder, adding primary water to restore into emulsion, accurately and quantitatively adding chlorate and perchlorate solution, and homogenizing under high pressure to obtain emulsion solution; step three, drying the emulsion solution in the step two in a spray dryer with low air inlet temperature to form milk powder; step four, drying the milk powder obtained in the step three in vacuum at a low temperature until the moisture content in the milk powder is not more than 2.0%. The invention also discloses an infant formula milk powder chlorate and perchlorate standard sample, which has the characteristics of uniformity, stability and accurate fixed value and can accurately and stably control the quality of the infant formula milk powder chlorate and perchlorate detection process.
Description
Technical Field
The invention belongs to the technical field of food detection, and particularly relates to a preparation method of an infant formula milk powder based chlorate and perchlorate standard sample and a prepared object standard sample.
Background
Chlorate is a disinfection by-product harmful to human bodies, perchlorate is a novel persistent chemical pollutant, and residual pollution of chlorate and perchlorate can be caused by pollution migration of cleaning and disinfecting nodes in the production of milk powder and milk powder packaging materials.
Chlorate and perchlorate are detected from infant formula powder of a plurality of brands in countries such as America, Germany and the like, and the two substances can obstruct the synthesis and secretion of thyroxine in human bodies, cause metabolism dysfunction and influence the normal growth and development of nerve centers of infants and young children. The world health organization sets the daily safe dosage of chlorate and perchlorate in food in 2007, and the national food and drug administration of China incorporates the chlorate and perchlorate into the risk monitoring project of infant formula powder in 2018. At present, chlorate and perchlorate are detected in China according to a method of BJS201706 'determination of chlorate and perchlorate in food'. However, a quality control method for detecting the content of infant formula milk powder chlorate and perchlorate is still lacked in China at present, and whether the detection process of the existing chlorate and perchlorate detection method is controlled, whether the personnel operation in the detection process is standard and the like cannot be examined and analyzed, so that whether the detection result (namely, chlorate and perchlorate content value) obtained by the detection method is accurate and reliable cannot be judged.
Disclosure of Invention
The inventor discovers that the content of chlorate and perchlorate in infant formula milk powder can be detected difficultly and the numerical value has deviation due to the fact that infant formula milk powder based standard samples with accurate and stable content are researched and used as quality control samples in a method for determining chlorate and perchlorate in food. Therefore, a first object of the present invention is to provide a method for preparing an infant formula milk powder-based chlorate and perchlorate standard sample, so as to obtain an infant formula milk powder-based chlorate and perchlorate standard sample with uniformity and stability, and ensure accurate and reliable content detection of chlorate and perchlorate. The second purpose of the invention is to provide a baby formula milk powder-based chlorate and perchlorate standard sample. The infant milk powder base chlorate and perchlorate standard sample can be applied to laboratory analysis method verification and analysis capability assessment of chlorate and perchlorate content detection, can also provide guarantee for milk powder detection technology research of detection institutions and quality safety risk analysis of infant milk powder enterprises, and can also provide scientific and fair basis and technical support for government supervision. The third purpose of the invention is to provide the application of the infant formula powder-based chlorate and perchlorate standard sample in quality control in the chlorate and perchlorate detection process of infant formula powder.
In order to achieve the purpose, the invention provides the following technical scheme:
the first purpose of the invention is to provide a preparation method of a standard sample of infant formula powder chlorate and perchlorate, which comprises the following steps:
step one, preparation of chlorate and perchlorate solution
Accurately weighing high-purity sodium chlorate and high-purity sodium perchlorate to 0.0001 g, and adding the high-purity sodium chlorate and high-purity sodium perchlorate into primary water to prepare chlorate and perchlorate solution;
step two, preparation of chlorate and perchlorate concentration in matrix emulsion powder
Quantitatively weighing matrix emulsion powder, adding primary water to restore into emulsion, accurately and quantitatively adding chlorate and perchlorate solution, and homogenizing under high pressure to uniformly disperse chlorate and perchlorate in the emulsion to obtain emulsion solution;
step three, spray drying at low air inlet temperature: drying the emulsion solution in the step two in a spray dryer with low air inlet temperature to form milk powder;
step four, vacuum drying: and (5) drying the milk powder obtained in the third step at low temperature in vacuum until the moisture content in the milk powder is not more than 2.0%.
According to the invention, the matrix milk powder is the matrix milk powder which meets the national standard GB 10767-2010 national standard for food safety of large infants and infant formula and GB 10765-2010 national standard for food safety of infant formula.
According to the invention, the primary water of the first step and the secondary step is the primary water specified in GB/T6682.
According to the invention, the pressure of the high-pressure homogenization in the second step is 100 MPa.
Further, the temperature of vacuum drying in the fourth step is 45-70 ℃, and the vacuum degree is 0.08-0.09 MPa.
Preferably, the temperature of vacuum drying in step four is 45 ℃.
According to the invention, the preparation method of the infant formula powder chlorate and perchlorate standard sample further comprises the following steps: step five, subpackaging: and D, quantitatively subpackaging the milk powder prepared in the step four into aluminum foil bags, filling nitrogen, and then carrying out heat sealing.
According to the invention, the preparation method of the infant formula powder chlorate and perchlorate standard sample further comprises the following steps: step six, content and uniformity inspection: and D, randomly sampling the milk powder obtained in the fifth step, and performing chlorate and perchlorate content detection and uniformity inspection to meet the requirements of standard samples.
According to the invention, the preparation method of the infant formula powder chlorate and perchlorate standard sample further comprises the following steps: step seven, stability monitoring: and D, storing the milk powder-based chlorate and perchlorate standard substances qualified in the step six in a dark place, and monitoring the short-term stability and the long-term stability at room temperature at the gradient temperature.
Further, the gradient temperatures for short-term stability monitoring were-25 deg.C, 0 deg.C, 20 deg.C, and 40 deg.C, respectively.
Further, the time for short term stability monitoring was 1 week.
Further, the time for long-term stability monitoring was 1 year, and the time for long-term stability monitoring was 0, 0.5, 1, 3, 6, and 12 months of room temperature.
As a second aspect of the invention, the infant formula milk powder-based chlorate and perchlorate standard sample is prepared by the preparation method.
As a third aspect of the present invention, an application of the above-mentioned infant formula powder-based chlorate and perchlorate standard sample in quality control in a chlorate and perchlorate detection process in infant formula powder is provided.
The invention has the beneficial effects that:
1. the infant formula milk powder chlorate-based perchlorate and perchlorate standard sample obtained by the preparation method has the characteristics of uniformity, stability and accurate fixed value, can accurately and stably control the quality of the detection process of the infant formula milk powder chlorate and perchlorate, and can be applied to laboratory analysis capability assessment and the research of the infant formula milk powder detection method; the content range of the standard sample is wide, and the standard sample is suitable for detecting the infant formula milk powder-based chlorate and perchlorate in different chlorate and perchlorate pollution conditions.
2. By adopting the composite technology of low air inlet temperature spray drying and vacuum drying, about 2 percent of milk powder finished products can be obtained, the content of the finished products of chlorate and perchlorate is matched with the design value, meanwhile, coke powder is not easy to form in the spray drying process, and the chlorate and perchlorate can uniformly and stably exist in the finished products.
Detailed Description
The present invention will be further described with reference to the following examples. It should be understood that the following examples are illustrative only and are not intended to limit the scope of the present invention. The experimental methods in the following examples, which are not specified under specific conditions, are generally carried out under conventional conditions.
1. Base milk powder of the following examples
The contents of chlorate and perchlorate in the matrix milk powder are accurately measured according to BJS201706 'determination of chlorate and perchlorate in food' respectively 20.2 mug/kg and 11.9 mug/kg.
It should be noted that the content difference of chlorate and perchlorate in the commercially available matrix milk powder is large, and the content of chlorate and perchlorate in the matrix milk powder selected by the invention is relatively low. Meanwhile, the matrix milk powder of the embodiment of the invention can be derived from the matrix milk powder which is in the market and meets the national standard GB 10767-.
2. Preparation of chlorate Standard solution and perchlorate Standard solution of the following examples
0.128 g of sodium chlorate (CAS:7775-09-9, purity > 99%) and 0.123 g of sodium perchlorate (CAS:7601-89-0) are respectively and accurately weighed into a volumetric flask of 1000ml after constant weight, and primary water specified by GB/T6682 is added to the volumetric flask to reach the fixed volume to the scale. After sealing, oscillating for 30 minutes, and preparing chlorate standard solution and perchlorate standard solution with the concentration of 100mg/L (counted by chlorate radical and perchlorate radical).
3. Pre-prepared low-concentration infant formula milk powder chlorate-based perchlorate standard sample and high-concentration infant formula milk powder chlorate-based perchlorate standard sample
(1) Low-concentration infant formula milk powder-based chlorate and perchlorate standard samples: the chlorate content is 70 mug/kg, and the perchlorate content is 20 mug/kg;
according to calculation, 50 microliters of chlorate solution and 8 microliters of perchlorate solution are required to be added into each hundred grams of milk powder base prepared by the milk powder base standard sample with the chlorate content of 70 micrograms/kg and the perchlorate content of 20 micrograms/kg.
(2) High-concentration infant formula milk powder-based chlorate and perchlorate standard samples: the chlorate content is 200 mug/kg, and the perchlorate content is 100 mug/kg;
according to calculation, 180 microliters of chlorate solution and 88 microliters of perchlorate solution are required to be added into every hundred grams of the milk powder base for preparing the milk powder base standard sample with the chlorate content of 200 micrograms/kg and the perchlorate content of 100 micrograms/kg.
Example 1 preparation of Low-concentration infant formula powder chlorate-based perchlorate standard sample
Accurately weighing 500.00 g of matrix milk powder, adding 1000.0 ml of primary water specified in GB/T6682, stirring and dissolving, adding 250 microliters of chlorate solution and 40 microliters of perchlorate solution, homogenizing for 2 times under 100MPa high pressure, and stirring the emulsion uniformly.
Spray drying at 130 deg.C to obtain milk powder containing chlorate and perchlorate with water content of 5.3%; drying at 45 deg.C and vacuum degree of 0.09MPa for 24 hr to obtain milk powder containing chlorate and perchlorate with water content of 1.8%.
Through detection, the obtained low-concentration infant formula milk powder chlorate and perchlorate standard sample are matched with preset concentrations (chlorate content is 70 mug/kg, perchlorate content is 20 mug/kg), and the preparation process is successful.
Example 2 preparation method of Low-concentration infant formula powder chlorate-based perchlorate standard sample
Accurately weighing 500.00 g of matrix milk powder, adding 1000.0 ml of primary water specified in GB/T6682, stirring and dissolving, adding 250 microliters of chlorate solution and 40 microliters of perchlorate solution, homogenizing for 2 times under 100MPa high pressure, and stirring the emulsion uniformly.
Spray drying at 135 deg.C to obtain milk powder containing chlorate and perchlorate with water content of 4.8%; drying at 45 deg.C under 0.09MPa for 18 hr to obtain milk powder containing chlorate and perchlorate with water content of 1.7%.
Through detection, the obtained low-concentration infant formula milk powder based chlorate and perchlorate standard sample are matched with the preset concentration, and the preparation process is successful.
Example 3 preparation method of Low-concentration infant formula powder chlorate-based perchlorate standard sample
Accurately weighing 500.00 g of matrix milk powder, adding 1000.0 ml of primary water specified in GB/T6682, stirring and dissolving, adding 250 microliters of chlorate solution and 40 microliters of perchlorate solution, and homogenizing for 2 times at 100 MPa.
Spray drying at 140 deg.C to obtain emulsion powder containing chlorate and perchlorate with water content of 4.2%; drying at 45 deg.C under 0.09MPa for 15 hr to obtain milk powder containing chlorate and perchlorate with water content of 1.5%.
Through detection, the obtained low-concentration infant formula milk powder based chlorate and perchlorate standard sample are matched with the preset concentration, and the preparation process is successful.
Comparative example 1 preparation method of standard sample of low-concentration infant formula milk powder-based chlorate and perchlorate
Accurately weighing 500.00 g of matrix milk powder, adding 1000.0 ml of primary water specified in GB/T6682, stirring and dissolving, adding 250 microliters of chlorate solution and 40 microliters of perchlorate solution, and homogenizing for 2 times at 100 MPa.
Spray drying at 170 deg.C to obtain emulsion powder containing chlorate and perchlorate with water content of 2.0%.
Through detection, the chlorate content and the perchlorate content in the standard sample of the low-concentration infant formula milk powder chlorate and the perchlorate are respectively 61.5 mu g/kg and 25.4 mu g/kg. The amount of chlorate is lower than the designed amount, while the amount of perchlorate is higher.
And (4) conclusion: the adoption of higher air inlet temperature can lead the chlorate content in the prepared finished product to be lower and the perchlorate to be higher. Moreover, coke powder is easily produced during the spray drying process. Therefore, the preparation process is not suitable for preparing low-concentration infant formula powder chlorate and perchlorate standard samples, and subsequent uniformity and stability tests are not continuously carried out.
Example 4 homogeneity test of Low-concentration infant formula chlorate, perchlorate standards
The powdered milk of examples 1-3 was dispensed in a unit of 8 g, heat-sealed with nitrogen, and 10 samples were randomly sampled and examined.
The uniformity of the prepared standard sample is tested by adopting a one-factor variance analysis method F test method, and F is obtained by checking an F distribution critical value table according to the significance level alpha of 0.05 and the degree of freedom (9,10)0.05(9,10) ═ 3.02, and F values of chlorate and perchlorate tested were 0.444 and 1.15, respectively, FA<F0.05(9,10) shows that there was no significant difference between the groups and the samples were homogeneous. The results are shown in tables 1 and 2.
TABLE 1 infant formula milk powder sample chlorate (Low concentration) uniformity test data (result unit: μ g/kg)
TABLE 2 infant formula milk powder sample perchlorate (Low concentration) homogeneity test data (result unit: μ g/kg)
Example 5 stability monitoring of Low concentration infant formula chlorate, perchlorate standards
The powdered milk of examples 1-3 was dispensed in a unit of 8 g, heat-sealed with nitrogen, and 20 samples were randomly sampled and examined.
The linear regression trend analysis t test method is adopted to carry out the short-term stability monitoring at the gradient temperature of-25 ℃, 0 ℃, 20 ℃ and 40 ℃ for 1 week and the long-term stability monitoring at the room temperature of 0, 0.5, 1, 3, 6 and 12 months, and the results meet the condition that the | b1 | is less than t |(0.95，n-2)·s(b1)。
(1) Short term stability monitoring data and statistics are shown in tables 3 and 4.
TABLE 3 infant formula milk powder sample chlorate (low concentration) short-term stability test results
TABLE 4 infant formula milk powder sample perchlorate (low concentration) short-term stability test results
(2) The long-term stability monitoring data and statistical results are shown in tables 5-8.
TABLE 5 Long-term stability test results of chlorate (low concentration) as standard sample of infant formula milk powder
TABLE 6 infant formula milk powder physical standard chlorate (low concentration) long-term stability test Linear fitting and statistical parameters
| b0 | |b1| | s | s(b1) | t(0.95,4) | t(0.95,4)*s(b1) | St | StSquare of | Significance of |
| 69.18 | 0.0349 | 0.382 | 0.0240 | 2.78 | 0.0689 | 0.29 | 0.08 | Whether or not |
TABLE 7 Long-term stability test results for perchlorate (low concentration) as standard sample of infant formula milk powder
TABLE 8 infant formula milk powder physical standard sample perchlorate (low concentration) long term stability test Linear fitting and statistical parameters
| b0 | |b1| | s | s(b1) | t(0.95,4) | t(0.95,4)*s(b1) | St | StSquare of | Significance of |
| 19.67 | 0.00491 | 0.186 | 0.0114 | 2.78 | 0.0317 | 0.14 | 0.02 | Whether or not |
The results show that the standard samples of examples 1 to 3 are stably preserved in short-term transportation and do not have a long-term tendency to change within 12 months.
Example 6 preparation of high concentration infant formula powder chlorate, perchlorate standards
Accurately weighing 500.00 g of matrix milk powder, adding 1000.0 ml of primary water specified in GB/T6682, stirring for dissolving, adding 900 microliters of chlorate solution and 440 microliters of perchlorate solution, and homogenizing for 2 times at 100MPa high pressure.
Spray drying at 130 deg.C to obtain milk powder containing chlorate and perchlorate with water content of 5.2%; drying at 45 deg.C and vacuum degree of 0.09MPa for 24 hr to obtain milk powder containing chlorate and perchlorate with water content of 1.8%.
Example 7 preparation of high concentration infant formula powder chlorate, perchlorate standards
Accurately weighing 500.00 g of matrix milk powder, adding 1000.0 ml of primary water specified in GB/T6682, stirring for dissolving, adding 900 microliters of chlorate solution and 440 microliters of perchlorate solution, and homogenizing for 2 times at 100MPa high pressure.
Spray drying at 135 deg.C to obtain milk powder containing chlorate and perchlorate with water content of 4.6%; drying at 45 deg.C under 0.09MPa for 18 hr to obtain milk powder containing chlorate and perchlorate with water content of 1.6%.
Example 8 preparation of high concentration infant formula powder chlorate, perchlorate standards
Accurately weighing 500.00 g of matrix milk powder, adding 1000.0 ml of primary water specified in GB/T6682, stirring for dissolving, adding 900 microliters of chlorate solution and 440 microliters of perchlorate solution, and homogenizing for 2 times at 100MPa high pressure.
Spray drying at 140 deg.C to obtain emulsion powder containing chlorate and perchlorate with water content of 4.0%; drying at 45 deg.C under 0.09MPa for 15 hr to obtain milk powder containing chlorate and perchlorate with water content of 1.4%.
Through detection, the obtained high-concentration infant formula milk powder based chlorate and perchlorate standard sample are matched with the preset concentration, and the preparation process is successful.
Comparative example 2 preparation method of high-concentration infant formula milk powder-based chlorate and perchlorate standard substance
Accurately weighing 500.00 g of matrix milk powder, adding 1000.0 ml of primary water specified in GB/T6682, stirring and dissolving, adding 250 microliters of chlorate solution and 40 microliters of perchlorate solution, and homogenizing for 2 times at 100 MPa.
Spray drying at 170 deg.C to obtain milk powder containing chlorate and perchlorate with water content of 1.8%.
Through detection, the chlorate and perchlorate contents in the standard sample of the high-concentration infant formula milk powder chlorate and perchlorate are 189 mug/kg and 113 mug/kg respectively. The amount of chlorate is lower than the designed amount, while the amount of perchlorate is higher. Therefore, the preparation process is not suitable for preparing high-concentration infant formula powder chlorate and perchlorate standard samples, and subsequent uniformity and stability tests are not continuously carried out.
Example 9 homogeneity test for high concentration infant formula chlorate, perchlorate standards
And subpackaging the milk powder by taking 8 g as a packaging unit, filling nitrogen, carrying out heat sealing, and randomly extracting 10 samples for inspection.
The uniformity of the prepared standard sample is tested by adopting a one-factor variance analysis method F test method, and F is obtained by checking an F distribution critical value table according to the significance level alpha of 0.05 and the degree of freedom (9,10)0.05(9,10) ═ 3.02, and F values of chlorate and perchlorate tested were 1.49 and 1.26, respectively, FA<F0.05(9,10) shows that there was no significant difference between the groups and the samples were homogeneous. Specifically, the results are shown in tables 9 and 10.
TABLE 9 infant formula milk powder sample chlorate (high concentration) uniformity test data (result unit: μ g/kg)
TABLE 10 infant formula milk powder sample perchlorate (high concentration) homogeneity test data (result unit: μ g/kg)
Example 10 stability monitoring of high concentration infant formula chlorate, perchlorate standards
The powdered milk of examples 1-3 was dispensed in a unit of 8 g, heat-sealed with nitrogen, and 20 samples were randomly sampled and examined.
Using linear loopsAccording to the trend analysis t test method, the short-term stability of 1 week at the gradient temperature of-25 ℃, 0 ℃, 20 ℃ and 40 ℃ and the long-term stability monitoring of the room temperature of 0, 0.5, 1, 3, 6 and 12 months are carried out, and the results meet the condition that b1 | < t |(0.95，n-2)·s(b1)。
(1) Short-term stability monitoring data and statistical results are shown in 11-12.
TABLE 11 infant formula milk powder physical standard chlorate (high concentration) short-term stability test results
TABLE 12 infant formula milk powder sample perchlorate (high concentration) short term stability test results
(2) The long-term stability monitoring data and statistical results are shown in tables 13-16.
TABLE 13 Long-term stability test results of chlorate (high concentration) as standard sample of infant formula milk powder
TABLE 14 infant formula milk powder physical standard chlorate (high concentration) long-term stability test Linear fitting and statistical parameters
| b0 | |b1| | s | s(b1) | t(0.95,4) | t(0.95,4)*s(b1) | St | StSquare of | Significance of |
| 199.30 | 0.124 | 1.12 | 0.0690 | 2.78 | 0.192 | 0.83 | 0.68 | Whether or not |
TABLE 15 Long-term stability test results of perchlorate (high concentration) as standard sample of infant formula milk powder
TABLE 16 infant formula milk powder physical Standard sample perchlorate (high concentration) Long-term stability test Linear fitting and statistical parameters
| b0 | |b1| | s | s(b1) | t(0.95,4) | t(0.95,4)*s(b1) | St | StSquare of | Significance of |
| 98.76 | 0.0248 | 0.761 | 0.0466 | 2.78 | 0.130 | 0.56 | 0.31 | Whether or not |
The results show that the standard samples of examples 6 to 8 are stably preserved in short-term transportation and do not have a long-term tendency to change within 12 months.
EXAMPLE 11 milk powder based chlorate, perchlorate standards chlorate, chlorate content rating
The standard samples of examples 1-3 and 6-8 were rated by using a combination of 8 institutions (Sichuan province food and drug inspection and testing institute, Zhejiang province food and drug inspection and testing institute, Doudou food and drug inspection and testing institute, Shanghai food and drug inspection institute, China inspection and certification group Shanghai Co., Ltd., Zhongke (Shanghai) testing technology Co., Ltd., Shanghai food research institute, and Nemontage Yili industry group GmbH), wherein the chlorate and the perchlorate content in the low-concentration infant formula milk powder chlorate and the perchlorate standard sample were respectively 70.9 + -7.0 μ g/kg and 19.4 + -1.9 μ g/kg, and the chlorate and the perchlorate content in the high-concentration infant formula milk powder chlorate and the perchlorate standard sample were respectively 204 + -10 μ g/kg and 96.4 + -3.4 μ g/kg.
Example 12 practical application of infant formula powder chlorate and perchlorate standards
(1) Existing detection procedures
Chlorate and perchlorate are detected according to a method of BJS201706 'determination of chlorate and perchlorate in food' of infant formula milk powder sold under the market brands in 1 section, 2 section and 3 section. No accompanying object standard sample exists in the pretreatment extraction and machine-loading processes, and the detection results are shown in Table 17.
TABLE 17 determination of chlorate and perchlorate content in 1, 2 and 3 stages of infant formula milk powder
| Chlorate mu g/kg | Perchlorate μ g/kg | |
| Infant formula 1-segment milk powder | 45.6 | 198 |
| Infant formula 2-segment milk powder | 59.5 | 232 |
| Infant formula 3-segment milk powder | 66.3 | 212 |
The results show that the results of perchlorate are higher than those of conventional infant formula powder, and the results are still between 190 and 230 mu g/kg after repeated tests.
And (4) analyzing results: the perchlorate content of the infant milk powder is generally 20-100 mug/kg, and the perchlorate contents of the three milk powders are abnormal, so that the phenomenon can be analyzed, on one hand, the perchlorate content of the milk powder is high, and on the other hand, problems possibly existing in the detection process are also checked.
(2) Detection of standard sample with infant formula milk powder-based chlorate and perchlorate
Chlorate and perchlorate are detected according to a method of BJS201706 'determination of chlorate and perchlorate in food' in section 1, section 2 and section 3 of the brand infant formula milk powder. The following material standard samples were taken in during the pretreatment extraction and the machine-up process, and the test results are shown in Table 18.
TABLE 18 determination of chlorate and perchlorate content in 1, 2 and 3 stages of infant formula milk powder
| Chlorate mu g/kg | Perchlorate μ g/kg | |
| Infant formula 1-segment milk powder | 46.7 | 189 |
| Infant formula 2-segment milk powder | 58.1 | 221 |
| Infant formula 3-segment milk powder | 65.1 | 210 |
| Standard sample (Low concentration) | 69.7 | 193 |
| Standard sample (high concentration) | 203 | 265 |
The result shows that the detection results of the low concentration and the high concentration of the standard sample chlorate in the object are both in the characteristic value range (the low concentration is 70.9 +/-7.0 mu g/kg, the high concentration is 204 +/-10 mu g/kg), the result of the simultaneous treatment of the milk powder chlorate of the sample to be detected is proved to be controllable, the detection results of the low concentration and the high concentration of the standard sample perchlorate in the object are both beyond the characteristic value range (the low concentration is 19.4 +/-1.9 mu g/kg, the high concentration is 96.4 +/-3.4 mu g/kg), and the problem is proved to occur in a certain link in the detection process, so that the result of the perchlorate is abnormal, and the reason needs to be found. The reason is found that the extracting solution is polluted by perchlorate, so that the sample is polluted in the extracting process.
After the extraction solution was replaced, the sample was tested again, and the following standard sample was taken in during the pretreatment extraction and the machine-up process, and the test results are shown in Table 19.
TABLE 19 content detection of chlorate and perchlorate in 1, 2 and 3 stages of infant formula milk powder
| Chlorate mu g/kg | Perchlorate μ g/kg | |
| Infant formula 1-segment milk powder | 45.6 | 15.8 |
| Infant formula 2-segment milk powder | 59.5 | 58.7 |
| Infant formula 3-segment milk powder | 66.3 | 35.5 |
| Standard sample (Low concentration) | 70.5 | 19.5 |
| Standard sample (high concentration) | 201 | 96.9 |
After the extracting solution is replaced, the detection result of the perchlorate is recovered to be normal, and the detection results of the perchlorate with low concentration and high concentration of the standard sample are both in the range of characteristic values, which shows that the detection process is not abnormal, and the detection results of 3 milk powders are accurate and reliable.
Example 13 example validation of infant formula powder based chlorate, perchlorate standards
(1) Artificially, the chlorate and perchlorate standard solutions used for detection were wrongly prepared (the standard curve concentration is doubled).
Detecting the infant formula 2-stage milk powder of a commercially available brand, and detecting chlorate and perchlorate according to a method of BJS201706 'determination of chlorate and perchlorate in food'. The following material standard samples were taken in during the pre-treatment extraction and machine-up process, and the test results are shown in table 20.
TABLE 20 content test of chlorate and perchlorate in 1, 2 and 3 stages of infant formula milk powder
| Chlorate mu g/kg | Perchlorate μ g/kg | |
| Infant formula 2-segment milk powder | 27.8 | 12.5 |
| Standard sample (Low concentration) | 36.5 | 9.52 |
| Standard sample (high concentration) | 96.4 | 50.1 |
The result shows that although no obvious abnormality is seen in the infant formula 2 section milk powder, the characteristic values of the accompanying standard sample chlorate and perchlorate (the chlorate is 70.9 +/-7.0 mu g/kg at low concentration, 204 +/-10 mu g/kg at high concentration, 19.4 +/-1.9 mu g/kg at low concentration and 96.4 +/-3.4 mu g/kg at high concentration) are much lower, and the abnormality is suggested to appear in the detection process.
(2) Detecting again after preparing standard solution normally
Chlorate and perchlorate are detected according to a method of BJS201706 'determination of chlorate and perchlorate in food' of the formula 2 section milk powder for the brand infants. The following material standard samples were taken in during the pretreatment extraction and machine-up processes, and the test results are shown in table 21.
TABLE 21 content detection of chlorate and perchlorate in 1, 2 and 3 stages of infant formula milk powder
| Chlorate mu g/kg | Perchlorate μ g/kg | |
| Infant formula 2-segment milk powder | 58.5 | 25.8 |
| Standard sample (Low concentration) | 69.5 | 20.1 |
| Standard sample (high concentration) | 198 | 98.8 |
The results show that the content of chlorate and perchlorate of the accompanying standard sample is in the characteristic value range after the standard solution with the correct concentration is prepared. The detection process is not abnormal, and the detection result obtained in the process of the infant formula 2 section milk powder is accurate and reliable.
Claims (10)
1. A preparation method of a standard sample of infant formula milk powder-based chlorate and perchlorate is characterized by comprising the following steps:
step one, preparation of chlorate and perchlorate solution
Accurately weighing high-purity sodium chlorate and high-purity sodium perchlorate, and adding the high-purity sodium chlorate and high-purity sodium perchlorate into primary water to prepare chlorate and perchlorate solution;
step two, preparation of chlorate and perchlorate concentration in matrix emulsion powder
Quantitatively weighing matrix emulsion powder, adding primary water to restore into emulsion, accurately and quantitatively adding chlorate and perchlorate solution, and homogenizing under high pressure to uniformly disperse chlorate and perchlorate in the emulsion to obtain emulsion solution;
step three, spray drying at low air inlet temperature: drying the emulsion solution in the step two in a spray dryer with low air inlet temperature to form milk powder;
step four, vacuum drying: and (5) drying the milk powder obtained in the third step at low temperature in vacuum until the moisture content in the milk powder is not more than 2.0%.
2. The method for preparing infant formula milk powder based chlorate, perchlorate standard sample according to claim 1, wherein the matrix milk powder is the matrix milk powder which meets the national standard GB 10767-2010 food safety national Standard for older infants and toddler formula and GB 10765-2010 food safety national Standard infant formula.
3. The method for preparing infant formula milk powder chlorate, perchlorate standard sample according to claim 1, wherein the temperature of vacuum drying in step four is 45-70 ℃ and the vacuum degree is 0.08-0.09 MPa.
4. The method for preparing the infant formula milk powder chlorate-based perchlorate-perchlorate standard sample according to claim 1, further comprising the step five of subpackaging: and D, quantitatively subpackaging the milk powder prepared in the step four into aluminum foil bags, filling nitrogen, and then carrying out heat sealing.
5. The method for preparing infant formula powder chlorate, perchlorate standard sample according to claim 1 or 4, characterized by further comprising the steps six, content and uniformity test: and (4) randomly sampling the milk powder obtained in the fourth step or the fifth step, and performing content detection and uniformity inspection on chlorate and perchlorate.
6. The method for preparing infant formula powder chlorate, perchlorate standard sample according to claim 5, characterized by further comprising the step seven of stability monitoring: and D, storing the milk powder-based chlorate and perchlorate standard substances qualified in the step six in a dark place, and monitoring the short-term stability and the long-term stability at room temperature at the gradient temperature.
7. The method for preparing infant formula powder chlorate, perchlorate standard sample according to claim 6, characterized in that the gradient temperature of short-term stability monitoring is-25 ℃, 0 ℃, 20 ℃, 40 ℃ respectively; the time for short term stability monitoring was 1 week.
8. The method of claim 6, wherein the time for long term stability monitoring is 1 year, 0, 0.5, 1, 3, 6, 12 months.
9. An infant formula powder chlorate-based perchlorate standard sample prepared by the preparation method according to any one of claims 1 to 8.
10. Use of a creamer-based chlorate, perchlorate standard sample according to any of claims 1 to 8 for use in quality control in a process for chlorate and perchlorate detection in a creamer for an infant.
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