Method for detecting beta-stimulants in dairy products
A technology for stimulants and dairy products, applied in the field of detecting beta-stimulants in dairy products, can solve the problem that beta-stimulant detection methods need to be studied and other issues
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Embodiment 1
[0041] In this example, 24 beta-agonists were tested according to the following method:
[0042] 1. Weigh 10g (accurate to 0.001g) of the milk sample into a 50mL high-speed centrifuge tube, add 20mL of 0.1mol / L dilute hydrochloric acid solution, and shake for 16 hours at 37±1°C. Take out the ultrasonic wave for 10 min, let the sample cool down to room temperature, vortex, and centrifuge at 11000 r / min for 10 min at 4°C. Take 10mL of the supernatant in another centrifuge tube, first add 5mL of 0.1mol / L perchloric acid solution, then use the perchloric acid solution to fine-tune the pH to 1.0±0.2, centrifuge at 5000r / min for 5min, take the supernatant in another In a centrifuge tube, adjust the pH of the supernatant to 9.5±0.2 with 10 mmol / L NaoH solution. Add 15mL of ethyl acetate to shake for 10min, vortex mix, centrifuge at 5000r / min for 10min, take the upper organic phase in a test tube, add 10mL of tert-butyl methyl ether (TBME) to the lower aqueous phase, shake for 10min,...
Embodiment 2
[0083]1. Linear range
[0084] Dilute the 24 mixed standard intermediate solutions with blank matrix solution to a concentration series of 0.02ng / mL, 0.05ng / mL, 0.10ng / mL, 0.20ng / mL, 0.50ng / mL, 1.00ng / mL, 2.00ng / mL standard working curve. The calibration curve is shown in Table 4 below.
[0085] Table 4 Calibration curve parameters
[0086]
[0087]
[0088] 2. Detection limit
[0089] 2.1 Instrument detection limit
[0090] The detection limits of this method are as follows:
[0091] The calculation results according to formula (1) are shown in Table 5 below.
[0092] Table 5 Instrument detection limit
[0093]
[0094]
[0095] 2.2 Method detection limit
[0096] 2.2.1 According to the formula (1) (2), the calculation results are shown in the table below.
[0097] Table 6 method detection limit
[0098]
[0099]
[0100] 2.2.2 According to the formula (1) (2), the calculation results are shown in Table 7 below.
[0101] Table 7 method detection li...
Embodiment 3
[0125] Detect according to the method of embodiment 1, the difference is that step 1 is as follows:
[0126] Weigh 10g (accurate to 0.001g) of the milk sample into a 50mL high-speed centrifuge tube, add 20mL of 0.1mol / L dilute hydrochloric acid solution, and shake at 37±1°C for 16h. Take out the ultrasonic wave for 10 min, let the sample cool down to room temperature, vortex, and centrifuge at 11000 r / min for 10 min at 4°C. Take 10mL of the supernatant into another centrifuge tube, first add 5mL of 0.1mol / L perchloric acid solution, then use the perchloric acid solution to fine-tune the pH to 1.0±0.2, centrifuge at 5000r / min for 5min, take the supernatant in another In the centrifuge tube, adjust the pH of the supernatant to 9.5±0.2 with 10 mmol / L NaOH solution. Add 15 mL of a mixed reagent containing equal volumes of ethyl acetate and tert-butyl methyl ether for extraction, shake for 10 min, vortex to mix, centrifuge at 5000 r / min for 10 min, take the upper organic phase int...
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