Method for detecting sodium cyclamate in grape wine
A technology of sodium cyclamate and sodium sulfamate, which is applied in the field of wine testing, can solve problems affecting the accuracy of test results, etc., and achieve the goals of saving processing time, saving manpower, and improving detection limits and quantitation limits Effect
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Embodiment 1
[0052] A detection method for sodium cyclamate in wine, comprising the following detection steps:
[0053] S1: Sample Extraction
[0054] Weigh the wine sample to be tested, filter it through a 0.22um filter membrane, and use it as the solution to be determined;
[0055] S2: Instrument preparation
[0056] Liquid chromatography-mass spectrometer / mass spectrometer: equipped with electrospray (ESI) ion source;
[0057] Constant temperature water bath;
[0058] Analytical balance, sensitivity 0.1mg, 0.1g;
[0059] S3: Reagents and Materials
[0060] Methanol: chromatographically pure;
[0061] Preparation of 10mmol / L ammonium acetate solution: Weigh 0.78g of high-grade pure ammonium acetate, dissolve it in water to 1000mL, add acetic acid to adjust the pH value of the solution to 5.3-5.4, shake well and filter through a 0.22um filter membrane for later use;
[0062] Preparation of sodium cyclamate standard working solution: Weigh 0.0100g sodium cyclamate standard product, dis...
experiment example 1
[0080] 1# sample: 0.1mg / L cyclamate water standard sample (prepared with water);
[0081] 2# sample: 0.1mg / L cyclamate red wine label sample (prepared with blank red wine);
[0082] The above two samples were respectively selected as the sample solution for method confirmation, and the display results of the chromatogram overlay mode after the two samples were run were compared.
[0083] According to the liquid phase elution conditions of the national standard GB5009.97 method, the superimposed chromatograms of the two samples after running are shown in figure 1 ;
[0084] The results are shown in Table 4.
[0085]
[0086] The results showed that the final test result was 0.17mg / L, which was seriously distorted due to the great influence of the original wine matrix when the standard cyclamate was added to the original wine. At the same time, both samples have certain tailing phenomenon, and the retention time is also quite different. Therefore, the detection of cyclama...
experiment example 2
[0088] The elution gradient of the national standard GB5009.97 method is slowed down, the elution conditions are shown in Table 5, and the superimposed chromatogram after running is shown in figure 2 ;
[0089]
[0090] The results are shown in Table 6: After the 2# sample was run, the final test result was 0.14mg / L, which was quite different from the real value due to the large influence of the original wine matrix.
[0091]
PUM
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