Determination method of volatile N-nitrosamine in tobacco, tobacco products and smoke
A determination method and technology for tobacco products, applied in the field of tobacco chemical inspection, can solve the problems such as the need to improve the detection sensitivity, unfavorable simplified operation, etc., and achieve the effects of simplifying the pretreatment process, short processing time, and high detection sensitivity
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Embodiment 1
[0029] The determination method of volatile N-nitrosamines in smokeless tobacco products comprises the following steps:
[0030] 1) Pretreatment of samples
[0031] Preparation of sample extract: Weigh 1.0g of buccal (smoke-free) tobacco product (accurate to 0.1mg), put it into a 15mL centrifuge tube with stopper, and accurately add 1.0mL of sodium hydroxide solution with a concentration of 1.0mol / L , add 10mL of dichloromethane after full infiltration, put it on an ultrasonic generator (purchased from Kunshan Ultrasonic Instrument Co., Ltd., model: KQ-700DB) for ultrasonic extraction for 20min, ultrasonic power 700W, frequency 40kHz, after standing for 5min, place Centrifuge on a centrifuge for 5 minutes at a rotational speed of 10,000 rpm, remove the supernatant (ie, the organic phase) and pass it through a 0.22 μm nylon membrane to obtain the sample extract.
[0032] Dewatering and purification of the sample extract: Take 1mL of the filtrate and transfer it to a solution c...
Embodiment 2
[0047] The determination method of volatile N-nitrosamines in cigarette mainstream smoke comprises the following steps:
[0048] 1) Pretreatment of samples
[0049] Preparation of sample extract: According to the regulations of GB / T 19609-2004 and ISO 4387:2000, use a straight-line smoking machine to smoke 5 cigarettes, and place the filter disc that captures the total particle phase of mainstream smoke into the container. Add 15 mL of dichloromethane, place it on an ultrasonic generator (same as in Example 1) for ultrasonic extraction for 20 min, with ultrasonic power of 700 W, frequency of 40 kHz, and pass the extract through a 0.22 μm nylon membrane to obtain the sample extract.
[0050] Dewatering and purification of the sample extract: Take 1mL of the filtrate and transfer it to a solution containing 15mg GCB, 12.5mg PSA, 70mgMgSO 4 and 25mg NaCl in a 15mL stoppered centrifuge tube, placed on an oscillator to vibrate for 10min at a speed of 1000rpm, then placed in a cent...
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