Method for detecting residual quantity of 34 illegally-added medicines in weight-losing health food
A health food and illegally added technology, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of poor adaptability of the matrix, impact on physical health, and insufficient coverage of drug types, etc., and reduce the requirements and time of ultrasonic extraction. , The effect of high dissolution efficiency
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Embodiment 1
[0050] Prepare self-made extract in advance, mix 700mL methanol, 300mL acetone and 1mL octanol polyoxyethylene ether, heat to reflux for 30min, cool and airtightly store for later use.
[0051]Test a commercially available oil-based capsule health product (sample A); accurately weigh 5.00g of the sample into a 50mL plastic centrifuge tube, then add 30mL of self-made extract, and quickly mix it on a vortex shaker for 1min to make the sample Mix thoroughly. Ultrasonic extraction for 5min, centrifugation at 4000r / min for 5min, take 5mL of the supernatant and dry it with nitrogen at 40°C, reconstitute with 2mL of 5% acetonitrile aqueous solution and filter through a 0.22μm microporous membrane, and the filtrate is subjected to HPLC-MS / MS determination, the results are shown in Table 3.
[0052] The detection conditions of HPLC-MS / MS are: in the positive ion monitoring mode, the chromatographic conditions are: chromatographic column: Agilent ZORBAX SB-C18 column (100mm×2.1mm, 1.8...
Embodiment 2
[0056] Prepare self-made extract in advance, mix 700mL methanol, 300mL acetone and 1mL octanol polyoxyethylene ether, heat to reflux for 30min, cool and airtightly store for later use.
[0057] Test a commercially available granular health product (sample B); accurately weigh 5.00g of the sample into a 50mL plastic centrifuge tube, then add 30mL of self-made extract, and quickly mix it on a vortex shaker for 1min to make the sample completely Mix well. Ultrasonic extraction for 5min, centrifugation at 4000r / min for 5min, take 5mL of the supernatant and dry it with nitrogen at 40°C, reconstitute with 2mL of 5% acetonitrile aqueous solution and filter through a 0.22μm microporous membrane, and the filtrate is subjected to HPLC-MS / MS determination, the results are shown in Table 3.
[0058] The detection conditions of HPLC-MS / MS are: in the positive ion monitoring mode, the chromatographic conditions are: chromatographic column: Agilent ZORBAX SB-C18 column (100mm×2.1mm, 1.8μm)...
Embodiment 3
[0062] Prepare self-made extract in advance, mix 700mL methanol, 300mL acetone and 1mL octanol polyoxyethylene ether, heat to reflux for 30min, cool and airtightly store for later use.
[0063] Test a commercially available tablet-type health product (sample C); accurately weigh 5.00g of the sample into a 50mL plastic centrifuge tube, then add 30mL of self-made extract, and quickly mix it on a vortex shaker for 1min to make the sample Mix thoroughly. Ultrasonic extraction for 5min, centrifugation at 4000r / min for 5min, take 5mL of the supernatant and dry it with nitrogen at 40°C, reconstitute with 2mL of 5% acetonitrile aqueous solution and filter through a 0.22μm microporous membrane, and the filtrate is subjected to HPLC-MS / MS determination, the results are shown in Table 3.
[0064] The detection conditions of HPLC-MS / MS are: in the positive ion monitoring mode, the chromatographic conditions are: chromatographic column: Agilent ZORBAX SB-C18 column (100mm×2.1mm, 1.8μm); ...
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