Method for detecting four nitrosoamino acids in buccal cigarette by liquid chromatography-tandem mass spectrometry
A technology of tandem mass spectrometry and liquid chromatography, which is applied in the field of liquid chromatography-tandem mass spectrometry to detect four kinds of nitroso amino acids in snus. Positive, safe and efficient effect of pretreatment
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Embodiment 1
[0032] Weigh 1g of the gum-based sample into a 50mL extraction centrifuge tube, add 1mL of n-hexane to disperse the sample. Add 10 mL of deionized water containing the internal standard, vortex at 2500 rpm for 30 min, take 5 mL of the extract, add it to an ISOLUTE diatomaceous earth solid-phase supported liquid-liquid extraction column (BIOTAGE isolute SLE), and elute three times with 30 mL of ethyl acetate , 10 mL each time, collect the eluate, concentrate to dryness at 45°C, redissolve with 0.5 mL deionized water, and mix well. Finally, it was analyzed by liquid chromatography-tandem mass spectrometry (LC-MS / MS).
[0033] NSAR and NAZCA were not detected in the gum-based snus, but NMPA and NMBA were contained.
Embodiment 2
[0035]Weigh 1g of American-style wet smoke directly into a 50mL extraction centrifuge tube. Add 10 mL of deionized water containing an internal standard, vortex at 2500 rpm for 30 min, take 5 mL of the extract, add it to an ISOLUTE diatomaceous earth solid-phase supported liquid-liquid extraction column (BIOTAGEisolute SLE), and use 30 mL of ethyl acetate to elute three times. 10 mL each time, collect the eluate, concentrate to dryness at 45°C, redissolve with 0.5 mL deionized water, and mix well. Finally, it was analyzed by liquid chromatography-tandem mass spectrometry (LC-MS / MS). The test results of 4 American wet smoke are shown in Table 6.
[0036] The sample test result of table 6 nitroso amino acids (by dry weight, ng / g)
[0037]
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