Method for detecting illegally-added 42 chemicals in Chinese patent medicines and health care products simultaneously
A detection method and illegal addition technology, applied in the field of food safety and food safety detection, can solve problems such as difficult effective market supervision, incomplete screening, long detection cycle, etc., and achieve simple pre-treatment process, fast detection speed, and selectivity strong effect
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Embodiment 1
[0027] Example 1. Detection of illegally added chemicals in functional drinks
[0028] (1) Sample preparation
[0029] Accurately weigh 2.00g (±0.01g) of a blank beverage sample that does not contain chemicals into a volumetric flask, add about 4ml of methanol aqueous solution (v:v, 1:1), and mix in the mixed solution with a concentration of 50ng / g. Dalafil, Reddenafil, Reddenafil, Homosildenafil, Sildenafil, Pseudovardenafil, Hydroxyhomosildenafil, Aminotadalafil, Thioai Denafil was mixed, and the volume was adjusted to 10ml. After centrifugal filtration, it was passed through a 0.45 μm filter membrane into an injection bottle for determination by high performance liquid chromatography-high resolution liquid chromatography-mass spectrometer.
[0030] (2) The chromatographic separation conditions of the high performance liquid chromatography-high resolution mass spectrometer are shown in Table 1, the analytical column filler used is C18, and the column temperature is 30°C.
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Embodiment 2
[0039]On the basis of Example 1, further in this example, standard working solutions with mass concentrations of 10, 50, 75, 100.0, and 200.0 ng / mL were prepared, and the chromatographic peak area of the characteristic ion of the target was taken as the ordinate y , Draw the standard working curve with the concentration of the target substance as the abscissa x. All compounds had a good linear relationship in the range of 10-200ng / mL, and the correlation coefficient (r) was greater than 0.99. If the response value of the drug in the sample solution is not within the linear range of the instrument, it should be properly diluted to the corresponding concentration range.
[0040] To determine whether there is any illegally added chemical drug in the sample, the following conditions must be met: the retention time deviation of the target substance in the sample solution and the retention time of the standard solution is within ±2.5%; The deviation of the accurate mass of the se...
Embodiment 3
[0046] Example 3. Detection of illegally added chemical drugs in propolis capsules and functional drinks
[0047] The application of illegally added chemicals in propolis capsules and functional drinks were detected respectively. According to the following methods, the propolis capsules and functional drinks were processed respectively.
[0048] Propolis capsules: Accurately weigh 2.00g (±0.01g) of the contents of the capsules into a volumetric flask, add about 4ml of methanol aqueous solution (v:v, 1:1), vortex to mix and dissolve, dilute to 10ml, and place in an ultrasonic extractor , sonicated for 20 minutes, centrifugally filtered, and passed through a 0.45 μm filter membrane into a sampling bottle for determination by high performance liquid chromatography-high resolution liquid chromatography-mass spectrometer.
[0049] Functional beverages: Accurately weigh 2.00g (±0.01g) of the beverage into a volumetric flask, add about 4ml of methanol aqueous solution (v:v, 1:1), di...
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