Method of determining specific aromatic amine released by azodye in cigarette paper through bonded phase chromatography-tandem mass spectrometry
A technology of tandem mass spectrometry and convergence chromatography, which is applied in the field of determination of carcinogenic aromatic amines, can solve the problems that liquid chromatography cannot be separated well, qualitative ability is not as good as tandem mass spectrometry, and sensitivity and qualitative ability are poor, so as to achieve fast and simple sensitivity, Avoid matrix effect, high recovery effect
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example 1
[0036] 1. Instruments and reagents:
[0037] Tert-butyl methyl ether and methanol are chromatographic grade reagents, sodium hydroxide and sodium sulfate are analytical reagents; distilled water meets the requirements of first-grade water in GB / T 6682.
[0038] UPCs 2 -MS / MS quadrupole tandem mass spectrometer; water bath constant temperature oscillator; Swiss Mettler AE 163 electronic balance (sensitivity: 0.0001g).
[0039] 2. Sample handling:
[0040] Weigh 1.0 g sample (accurate to 0.0001 g); put the fragments in a 50 mL Erlenmeyer flask with a stopper, place the sample in a 50 mL stoppered centrifuge tube, add 15 mL of citric acid buffer preheated to 70±2°C Shake vigorously to soak the sample, and place it in a 70±2°C water bath for 30 minutes; add 3 mL of 200 mg / mL sodium dithionite aqueous solution, keep it at 70±2°C, react for 30 minutes, and then place the centrifuge tube in an ice-water bath Cool to room temperature within 2 minutes;
[0041] Add 0.5 mL of 40% ...
example 2
[0045] According to the determination method described in Example 1, another cigarette paper sample was selected, and the p-chloroaniline content in the sample was 2.25 mg / kg.
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