Method for measuring phthalate type compound content in reconstituted tobacco
A technology of phthalic acid and ester compounds, applied in the direction of measuring devices, instruments, scientific instruments, etc., to achieve the effects of improving sensitivity, reducing errors, and good repeatability
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Embodiment 1
[0035] The method for measuring the content of phthalates in reconstituted tobacco leaves in this embodiment is as follows (measurement method flow process is as follows: figure 1 shown)
[0036] 1. Preparation of internal standard solution:
[0037] Weigh 0.2g of benzyl benzoate, put it in a 10mL volumetric flask, dissolve it with ethanol and constant volume, and prepare an internal standard solution with a concentration of 20mg / mL; store the internal standard solution in a sealed refrigerator at 4°C, and the validity period is 3 moon;
[0038] 2. Configuration of standard working solution:
[0039] (1) Mixed standard stock solution I: Accurately weigh 100 mg of 7 kinds of phthalate compounds and place them in the same 100mL volumetric flask, dissolve them with ethanol and constant volume, and mix well to obtain mixed standard stock solution I, in which each The concentration of the components is 1mg / mL; the mixed standard stock solution I is sealed and stored in a refrige...
Embodiment 2
[0067] The method for determining the content of phthalates in reconstituted tobacco leaves in this embodiment is as follows
[0068] 1. Preparation of sample solution to be tested
[0069] Place the reconstituted tobacco leaf sample on a balance and weigh it, then cut it into pieces no larger than 0.5cm×0.5cm, place it in a 50mL Erlenmeyer flask with a stopper, add 20mL of isopropanol solution and 10μL of internal standard solution, ultrasonically extract for 30min, and statically After the extract is cooled to room temperature, pipette 2.0 mL of the supernatant to pass through a 0.45 μm organic filter membrane to prepare the sample solution to be tested;
[0070] 2, adopt the chromatographic mass spectrometry condition in the embodiment 1 to analyze the sample solution to be tested;
[0071] 3, will measure the chromatographic peak area ratio of 7 kinds of phthalates and internal standard, substitute into the standard curve drawn in embodiment 1, obtain the content of phtha...
Embodiment 3
[0076] The present embodiment is as follows to the detection method of the repeatability of the inventive method and the standard addition recovery rate:
[0077] Add each phthalate standard sample of 3 different concentrations of high, middle and low respectively in the sample, measure 5 times respectively for each sample, the chromatography mass spectrometry analysis condition is the same as the chromatography mass spectrometry analysis condition of embodiment 1, calculate this method according to the analysis result The recovery rate of phthalates in the reconstituted tobacco leaves and the relative standard deviation of the measured value after the standard addition, the results are shown in Table 5;
[0078] Table 5 The recovery rate and standard deviation of the addition of phthalates in reconstituted tobacco leaves
[0079] Compound name
[0080] As can be seen from Table 5, the recoveries of the seven compounds are between 95% and 104%, and the average relati...
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