| Objective:This paper optimized two kinds of rapid analysis methods for 13 kinds of food additives.High performance liquid chromatography(HPLC),which is accurate,sensitive,reproducible and fast,can be used to detect many kinds of food additives at the same time.The chromatography of 13 kinds of food additives commonly six kinds of food detection method to improve,and using the method in Tianqiao District of Ji'nan City,the sale of food security status of the investigation and analysis,provide the basis for the establishment of market supervision measures.Method:1 Sampling By means of multi-stage,stratified random sampling method,six types of food,cakes,preserved candy,marinade,canned fruit,soda and drink and fruit wine are collected from Tianqiao district in 2015?2017;20 kinds of food of every type were sampled each year.2 Food additives measured Sorbic acid,benzoic acid,sodium saccharin,acesulfame,dehydroacetic acid,lemon yellow,amaranth red,new red,sunset yellow,indigo blue,brilliant blue,erythrosine,fancy red.3 Test methods Traditional detection methods were optimized,HPLC method with detector of PDA was used.The maximum absorption wavelengths of the additives are determined by spectrum scanning.With spectrogram analysis,mobile phase is adjusted and gradient elution condition was set up.Method validated,compared with the results from currently effective national standard method.By conventional way,precision,stability and recovery test were carried out,and showed a satisfactory result.The method is verified by linear relationship,precision and recovery test,and the results are compared with those of the national standard method,indicating that the test results meet the test requirements.4 Market survey Through investigation of 6 types of foods in Tianqiao District of Jinan,marketing survey by sampling detects the use of additives,according to the?GB2760-2014 standard provisions of the use of food additives?,the detection rate and the rate exceeding the standard results,provide a reference basis for the formulation of regulatory measures.5 Statistics Statistical processing uses Excel to establish a database.SPSS 18.0 was used for data analysis,and the comparison of inter group rates was checked with Chi-square test.Results:1 The two experimental methods established in this paper have a low detection limit,and the linear relationship between the chromatographic separation degree and the standard curve of the additive is in line with the requirements of the methodology.1.1 Acesulfame,benzoic acid,sorbic acid,sodium saccharin and dehydroacetic acid in 5 kinds of food additives,ranging 0.00?0.10 mg/mL,the correlation coefficient of each component of the curve is higher than 0.999,the relative standard deviation(RSD)of 0.87%?1,73%,the recoveries of the sample recovery rate was 97.0%?101.7%.1.2 New red,lemon yellow,amaranth,indigo,sunset yellow,bright blue and Allura red,erythrosine and other 8 kinds of food additives,the 8 components can be separated completely,showed a good linear relationship(R>0.999),the relative standard deviation was 0.90%?1.54%%,and the recovery rate was 91.0%?105.8%.2 Results of investigation and analysis of food additives2.1 Different annual detection results from 2015 to 2017 food additives detection rates were 68.3%,75.0%,79.2%,the trend was increasing year by year the difference was statistically significant(?2=0.0498,P<0.05);food additives exceed the standard rate of 48.3%(2015),41.7%(2016),43.3%(2017),the difference was not statistically significant(?2=1.1123,P>0.05).2.2 The test results of different food categories:six kinds of food are all different degrees of food additives,the existence of excessive standard use.Cakes and carbonated drinks in the detection rate was 100%,pickled products and additives were prepared with less alcohol;in addition to the cake and pastry exceed the standard rate was the highest for acesulfame,the remaining five categories of food are the highest exceed the standard rate of benzoic acid;benzoic acid is the main project exceed the standard six categories of food.2.3 The detection results of different kinds of food additives:the detection rate is from high to low in order of preservatives(29.1%),sweeteners(26.5%),synthetic colorants(12%),and the over standard rates from high to low are preservatives(19.7%),sweeteners(16.2%),synthetic colorants(8.5%).The detection rate and superstandard rate of preservatives were the highest,and the detection rate of benzoic acid was as high as 41.7%,and the rate of exceeding the standard was up to 33.3%.2.4 Different test results of the project:the highest detection rate for benzoic acid,sodium saccharin(38.6%)(31.9%)of sorbic acid(25%),dehydroacetic acid(23.6%)ace-k(21.1%)is also high,indigo and light blue the lowest detection rate(5.8%);the highest rate of benzene to exceed the standard(26.1%)benzoic acid,sorbic acid(18.9%times),acesulfame,sodium saccharin(16.7%)(15.8%),dehydroacetic acid(14.2%)is also high,bright blue(3.6%)exceed the standard rate is the lowest.2.5 Brand and nonbrand food test results:the total detection rate of brand products(32.8%)and the exceeding standard rate(23.9%)were significantly lower than the total detection rate of nonbrand products(68.3%)and the exceeding standard rate(34.4%).2.6 The detection results of different packaged foods were:the detection rate of stereotyped packaged foods(43.3%)and the exceeding standard rate(22.4%)were all lower than that of bulk food(68.7%)and the exceeding standard rate(28%).Conclusion:1 The optimized methods have several advantages:rapid preprocess,efficient extraction,good linearity for the standard curve,good precision and accuracy,which meet with the requirements for investigation.2 Ji'nan Tianqiao District,2015?2017,the detection rate of food additives showed an upward trend in the year of 2015?2017.The preservatives and sweeteners used widely in all kinds of foods.The major over-used category was benzoic acid.3 The problem of additive-exceeding of food additives in the farmers' market,nonbrand and bulk food is more serious. |
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