Method for simultaneous determination of benzbromarone, allopurinol and probenecid in health food
A technology of benzbromarone and health food, applied in the field of health food
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Embodiment 1
[0037] The method for simultaneously measuring the content of benzbromarone, allopurinol and probenecid in the health food provided by the present embodiment comprises the following steps:
[0038] (1) Sample pretreatment: Take a commercially available brand of solid powdered anti-gout health food as the sample to be tested, accurately weigh 2g of the sample after mixing thoroughly, put it in a 50mL centrifuge tube, add 10mL 0.1% ammonia water-acetonitrile (v / v) solution and 1gNaCl, vortex and mix for 1min, ultrasonic frequency is 40kHz, then ultrasonically extract for 5min, centrifuge at 8000r / min for 5min, collect the supernatant; add 10mL 0.1% ammonia water-acetonitrile (v / v) solution to the centrifuge tube and repeat the above extraction operation, combine the supernatant twice, add 150mg QuEChERS reagent (containing PSA powder and C 18 The powder ratio is 2:1) and 1g of anhydrous Na 2 SO 4 Purify, vortex mix for 3min, centrifuge at 8000r / min for 5min; pipette 5mL of sup...
Embodiment 2
[0061]Taking another brand of solid anti-gout health food on the market as the sample to be tested, the sample detection includes the following steps:
[0062] (1) Sample pretreatment, preparation of standard solution, detection and analysis are the same as in Example 1.
[0063] (2) Analysis of results
[0064] The liquid chromatography-tandem mass spectrogram (see figure 2 ) compared with the standard sample for qualitative analysis, the contents of the three drugs in the solid powder anti-gout health food were calculated by the standard curve, the same sample to be tested was repeatedly detected three times, and the average value was obtained. The test results are shown in Table 3.
Embodiment 3
[0066] Taking a commercially available brand of liquid anti-gout health food as the sample to be tested, the sample detection includes the following steps:
[0067] (1) Sample pretreatment: Accurately weigh 2 g of the sample after thorough mixing, place it in a 50 mL centrifuge tube, add 5 mL of 0.1% ammonia-acetonitrile (v / v) solution and 2 g of NaCl, vortex and shake for 1 min, and ultrasonic frequency 40kHz, then ultrasonically extract for 5min, centrifuge at 8000r / min for 5min, and collect the supernatant; add 5mL of 0.1% ammonia water-acetonitrile (v / v) solution to the centrifuge tube to repeat the above extraction operation, combine the supernatant twice, Add QuEChERS reagent and 1 g Na-free 2 SO 4 , vortexed for 3 minutes, centrifuged at 8000r / min for 5 minutes; pipette 5mL of the supernatant into a glass tube, dried with nitrogen at 40°C, and reconstituted with 1mL of 0.1% ammonia-acetonitrile (v / v); the supernatant The solution was passed through a 0.22μm filter mem...
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