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

Active Publication Date: 2017-12-01
GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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  • Method for simultaneous determination of benzbromarone, allopurinol and probenecid in health food
  • Method for simultaneous determination of benzbromarone, allopurinol and probenecid in health food
  • Method for simultaneous determination of benzbromarone, allopurinol and probenecid in health food

Examples

Experimental program
Comparison scheme
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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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Abstract

The invention discloses a method for simultaneous determination of benzbromarone, allopurinol and probenecid in health food, which comprises the following steps: (1) sample pretreatment; (2) standard solution preparation; (3) benzbromarone, allopurinol and probenecid content determination. In the method, a sample to be determined is purified by QuEChERS Extract after extraction with ammonia water-acetonitrile, and positive and negative ion-exchange scanning is performed by a HPLC-MS/MS method to solve the technical difficulty that the difference in the chemical properties of the benzbromarone, allopurinol and probenecid is large, so that simultaneous extraction and determination is difficult to realize, and also solve the problems that the health food matrix interference is serious, and the recovery rate is low; the method for online simultaneous determination of the content of the benzbromarone, allopurinol and probenecid in anti-gout health food is established, which fills the technical gap in simultaneous determination of the content of the benzbromarone, allopurinol and probenecid in the anti-gout health food.

Description

technical field [0001] The invention belongs to the technical field of health food, in particular to a method for simultaneously measuring the contents of benzbromarone, allopurinol and probenecid in health food. Background technique [0002] Gout is a chronic metabolic disorder caused by purine metabolism disorder. The clinical symptoms are mainly hyperuricemia, and urate crystallizes in the joints, kidneys and connective tissues, which can cause local inflammation of the joints and infiltration of granulocytes. Gout often recurs, lingering and difficult to heal. It is a lifelong disease. Its condition often alternates between acute and intermittent periods. If it is only treated in the acute period and not treated in the intermittent period, it will only make the attack repeated. And gradually increase the weight of, until serious adverse consequences are caused, so the key to the treatment of gout is to persist in treatment. In recent years, due to the aging of the popu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88G01N30/06G01N30/34
CPCG01N30/06G01N30/34G01N30/88G01N2030/884G01N2030/8845
Inventor 邓幸飞綦艳刘仲义李锦清刘辉郦明浩张燕孟维伟
Owner GUANGDONG TESTING INST OF PROD QUALITY SUPERVISION
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