Method for detecting six trace sweetening agents in white spirit by ultra-high pressure liquid chromatography and time-of-flight mass spectrometry
A technology of time-of-flight mass spectrometry and ultra-high pressure liquid phase, which is applied in measurement devices, instruments, scientific instruments, etc., can solve the problems that the detection sensitivity needs to be improved and cannot be dealt with, and achieves a simple and fast analysis method, high sensitivity and good selectivity. Effect
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example 1
[0062] The following example will specifically illustrate the operation method of the present invention, but can not be used as the limitation of the present invention. Example 1 Detection of sweeteners of a certain brand of liquor on the market
[0063] 1 material
[0064] 1.1 Instrument
[0065] Ultra-high pressure liquid chromatography: WATERS ACQUITY UPLC, detector: WATERS ACQUITYPDA, chromatographic column: BEH C-18 2.1mm×50mm 1.7um, time-of-flight mass spectrometer: WATERSSYNAPT MS, Masslynx 4.1 mass spectrometry management software.
[0066] 1.2 Reagents and samples
[0067] Methanol: chromatographically pure (Sinopharm Group); 20mmol / L ammonium acetate solution: Dissolve 1.54g of ammonium acetate (Sinopharm Group) with ultrapure water to 1000ml, and then filter through a 0.2μm filter membrane; six sweetener standard samples: saccharin Sodium, sodium cyclamate, acesulfame-K purity is 99.9% (Sigma company of the United States); Aspartame purity is 99.0% (Sigma company...
example 2
[0104] Example 2 Detection of sweeteners of a certain brand of liquor on the market
[0105] Detected another commercially available liquor sample in the same manner as in Example 1 above. In Example 2, pretreatment methods, chromatographic mass spectrometry conditions, detection instruments, and standard curves were all with reference to Example 1.
[0106] Result analysis
[0107] The chromatogram ( Figure 7 ) It can be seen that the retention time of sodium saccharin, one of the six sweeteners, is 2.43min, and the sample ( Figure 16 ) in 2.41min place has a chromatographic peak and the sodium saccharin chromatographic peak retention time is similar, therefore can preliminarily determine sample chromatogram ( Figure 16 ) The chromatographic peak at 2.41min is sodium saccharin. Then according to the sample at m / z=182 place characteristic molecular ion peak ( Figure 9 ), which is the same as the characteristic molecular ion peak of sodium saccharin ( Figure 17 ), it ...
example 3
[0110] Example 3 Detection of sweeteners of a certain brand of liquor on the market
[0111] Detected another commercially available liquor sample in the same manner as in Example 1 above. In Example 3, pretreatment methods, chromatographic mass spectrometry conditions, detection instruments, and standard curves were all with reference to Example 1.
[0112] Result analysis
[0113] The chromatogram ( Figure 7 ) It can be seen that the retention times of acesulfame-K, sodium saccharin, and cyclamate are respectively 1.75min, 2.43min, and 2.91min among the six sweeteners, and the samples ( Figure 18 ) in 1.73min, 2.43min, 2.91min chromatographic peaks can be preliminarily judged as three kinds of sweeteners of acesulfame potassium, saccharin sodium, sodium cyclamate, and then according to the sample at the corresponding retention time respectively m / z=162 ( Figure 19 ), m / z=178, m / z=182 characteristic molecular ion peaks are consistent with the characteristic molecular ion...
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