Detection method of 22 kinds of illegally added sedative drugs residues in health products
A technology of illegal addition and detection method, which is applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of single processing method, time-consuming, cumbersome operation, etc., and achieve the effect of improving detection efficiency, shortening time, and high dissolution efficiency
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Embodiment 1
[0046] Prepare self-made extract in advance, mix 1000g methanol, 100g ethyl acetate and 1g octanol polyoxyethylene ether, heat to reflux for 30min, cool and airtightly store for later use.
[0047] Test a commercially available capsule health product (sample A); accurately weigh 5.00g of the sample into a 50mL plastic centrifuge tube with stopper, then add 30mL of self-made extract, and quickly mix it on a liquid mixer for 1min to make the sample Mix thoroughly. Ultrasonic extraction for 5min, centrifugation at 4000r / min for 10min, 1mL supernatant was blown dry with nitrogen at 40°C, reconstituted with 1mL of 50% methanol aqueous solution; after filtering through a 0.22μm microporous membrane, the filtrate was subjected to HPLC-MS / MS determination, the results are shown in Table 3.
[0048]The detection conditions of HPLC-MS / MS are: the chromatographic conditions in the positive ion monitoring mode are: chromatographic column: Agilent RRHD SB-C18 column (100mm×2.1mm, 1.8μm);...
Embodiment 2
[0052] Prepare self-made extract in advance, mix 1000g of methanol, 100g of ethyl acetate and 1g of octanol polyoxyethylene ether, heat to reflux for 30min, cool and seal for storage until use.
[0053] Test a commercially available granular health product (sample B); accurately weigh 5.00g of the sample into a 50mL plastic centrifuge tube with stopper, then add 30mL of self-made extract, and quickly mix it on a liquid mixer for 1min to make the test Mix completely. Ultrasonic extraction for 5min, centrifugation at 4000r / min for 10min, 1mL supernatant was blown dry with nitrogen at 40°C, and reconstituted with 1mL of 50% methanol aqueous solution. After passing through a 0.22 μm microporous membrane, the filtrate was determined by HPLC-MS / MS, and the results are shown in Table 3.
[0054] The detection conditions of HPLC-MS / MS are: in the positive ion monitoring mode, the chromatographic conditions are: chromatographic column: Agilent RRHDSB-C18 column (100mm×2.1mm, 1.8μm); c...
Embodiment 3
[0058] Prepare self-made extract in advance, mix 1000g of methanol, 100g of ethyl acetate and 1g of octanol polyoxyethylene ether, heat to reflux for 30min, cool and seal for storage until use.
[0059] Test a commercially available tablet-type health product (sample C); accurately weigh 5.00g of the sample into a 50mL plastic centrifuge tube with stopper, then add 30mL of self-made extract, and quickly mix it on a liquid mixer for 1min to make The sample was mixed thoroughly. Ultrasonic extraction for 5min, centrifugation at 4000r / min for 10min, 1mL supernatant was blown dry with nitrogen at 40°C, and reconstituted with 1mL of 50% methanol aqueous solution. After passing through a 0.22 μm microporous membrane, the filtrate was determined by HPLC-MS / MS, and the results are shown in Table 3.
[0060] The detection conditions of HPLC-MS / MS are: in the positive ion monitoring mode, the chromatographic conditions are: chromatographic column: Agilent RRHDSB-C18 column (100mm×2.1mm...
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