Method for determining aflatoxin B1 in gardenia yellow
A technology of aflatoxin and gardenia yellow, applied in the field of food additives, can solve the problems of inaccurate qualitative, poor sensitivity and high detection limit, and achieve the effects of good repeatability, high sensitivity and high recovery rate
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Embodiment 1
[0047] With a volume fraction of 90% acetonitrile aqueous solution as a solvent, prepare aflatoxin B with concentrations of 0.1, 0.5, 1.0, 2.0, 5.0 μg / L 1 A series of standard solutions were detected by ultra-high performance liquid chromatography-tandem mass spectrometry, and quantified by external standard method. The specific operation is as follows:
[0048] High performance liquid chromatography-tandem mass spectrometry conditions are:
[0049] Column: BEH C 18 , 2.1×50mm, 1.7μm;
[0050] Column temperature: 40°C;
[0051] Mobile phase: 5mmol / L ammonium formate + 0.1% formic acid aqueous solution (mobile phase A) and acetonitrile (mobile phase B) as the mobile phase for gradient elution;
[0052] Flow rate: 0.4mL / min;
[0053] Injection volume: 5 μL;
[0054] The mass spectrometry conditions are:
[0055] Detection method: use mass spectrometer for multi-ion reaction monitoring;
[0056] Ionization method: ESI+;
[0057] Desolvation temperature: 450°C;
[0058] ...
Embodiment 2
[0073] (1) Weigh 10g gardenia yellow sample (without aflatoxin B 1 ) accurate to 0.01g, add aflatoxin B 1 Standard solution, with a concentration of 0.10 μg / kg, to obtain aflatoxin B-containing 1 For the gardenia yellow sample, put the sample in a 100mL beaker, dissolve it with 100mL of water and transfer the sample to a 250mL separatory funnel;
[0074] (2) Add 100mL of chloroform to the separatory funnel, shake vigorously, mix well, and keep still to separate layers;
[0075] (3) The lower layer solution was transferred to a 250mL round bottom flask, 50°C was rotated to dryness, and the round bottom flask was rinsed with 2mL volume fraction of 90% acetonitrile aqueous solution to obtain the eluate;
[0076] (4) The eluent is transferred to a solution containing 0.5g N-propylethylenediamine and 0.5g C 18 Centrifuge at a speed of 10000r / min for 10min in a packed centrifuge tube;
[0077] (5) After passing the above-mentioned centrifuged liquid through a 0.22 μm organic fil...
Embodiment 3
[0086] According to sample pretreatment method and instrumental analysis detection method in embodiment 2, to gardenia yellow sample (not containing aflatoxin B 1 ) Add aflatoxin B 1 Standard solution, for experiments with different spiked concentrations. Three spiked amounts were set, and the average value was measured three times for each sample with spiked content, and the spiked recovery rate of the sample was calculated according to the actual added amount and the measured results. The results are shown in Table 4. It can be seen from Table 4 that the recovery rate of the samples is in the range of 91.5-104%. The selected ion chromatogram with a spiked concentration of 0.20 μg / kg is as follows image 3 It can be seen from the figure that the retention time of aflatoxin in the gardenia yellow sample is stable, the linear relationship between the concentration and the response value is good, and the recovery rate of the target substance is ideal.
[0087] The recovery r...
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