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Method for detecting residue of 18 illegally-added blood-glucose-reducing and antihypertensive drugs in health product

A technology for illegal addition, lowering blood sugar and lowering blood pressure, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of unspecified testing methods and health impacts, and achieve the goal of reducing requirements, shortening time, and improving detection efficiency Effect

Active Publication Date: 2018-02-27
浙江公正检验中心有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Health care products currently on the market can be roughly divided into general health food, health medicine, health cosmetics, health care products, etc., while health care medicines are nutritious and food-based natural medicines, and should be used in conjunction with treatment, with usage and dosage requirements. Drugs with "healthy" batch numbers, but in order to increase marketing, many unscrupulous merchants directly add some illegally used drugs to health products to achieve specific medicinal effects, such as hypoglycemic drugs tolbutamide, glibenclamide, glibenclamide, Lizide and antihypertensive drugs atenolol, clonidine hydrochloride, etc.
The abuse of these drugs will have a serious impact on people's health. Therefore, it has certain social significance to establish an effective method for detecting the residues of illegally added hypoglycemic and antihypertensive drugs in health products.
[0003] According to the existing methods for detecting the residues of antidiabetic and antihypertensive drugs illegally added in health products, the existing national standards are only the State Food and Drug Administration Drug Inspection Supplementary Inspection Methods and Inspection Items Approval Document 2009029, the Supplementary inspection method and inspection item approval document 2009032, there is no specific inspection method yet

Method used

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  • Method for detecting residue of 18 illegally-added blood-glucose-reducing and antihypertensive drugs in health product
  • Method for detecting residue of 18 illegally-added blood-glucose-reducing and antihypertensive drugs in health product
  • Method for detecting residue of 18 illegally-added blood-glucose-reducing and antihypertensive drugs in health product

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] Prepare self-made extract in advance, mix 1000g of methanol, 100g of ethyl acetate and 1g of decyl alcohol polyoxyethylene ether, heat to reflux for 30min, cool and seal for storage until use.

[0046] 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, take 1mL of the supernatant and dry it with nitrogen at 40°C, reconstitute with 1mL of 5% acetonitrile aqueous solution; after passing through a 0.22μm microporous membrane, the filtrate is subjected to HPLC-MS / MS Determination, the results are shown in Table 3.

[0047] The detection conditions of HPLC-MS / MS are: the chromatographic conditions in the positive ion monitoring mode are: chromatographic column: Agilent ZORBAX SB-C18 column ...

Embodiment 2

[0051] Prepare self-made extract in advance, mix 1000g of methanol, 100g of ethyl acetate and 1g of decyl alcohol polyoxyethylene ether, heat to reflux for 30min, cool and seal for storage until use.

[0052] 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, take 1mL of the supernatant and dry it with nitrogen at 40°C, reconstitute with 1mL of 5% acetonitrile aqueous solution; after passing through a 0.22μm microporous membrane, the filtrate is subjected to HPLC-MS / MS Determination, the results are shown in Table 3.

[0053] 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 ...

Embodiment 3

[0057] Prepare self-made extract in advance, mix 1000g of methanol, 100g of ethyl acetate and 1g of decyl alcohol polyoxyethylene ether, heat to reflux for 30min, cool and seal for storage until use.

[0058] 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 5 minutes, centrifugation at 4000r / min for 10 minutes, 1 mL of the supernatant was blown dry with nitrogen at 40°C, and redissolved with 1 mL of 5% acetonitrile 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.

[0059] The detection conditions of HPLC-MS / MS are: in the positive ion monitoring mode, the chromatographic conditions are: chromatographic column: Agilent ZORB...

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Abstract

The invention relates to the technical field of drug residue detection and aims at providing a method for detecting residue of 18 illegally-added blood-glucose-reducing and antihypertensive drugs in ahealth product, which has the characteristics of rapidness, accuracy, simplicity and low cost. According to the technical scheme, the method for detecting the residue of the 18 illegally-added blood-glucose-reducing and antihypertensive drugs in the health product comprises the following steps: (1) preparing homemade extract, namely refluxing a mixture of methyl alcohol, ethyl acetate and decyl alcohol polyoxyethylene ether for 30 minutes at the temperature of 60-65 DEG C, and cooling for later use; (2) taking health product tablets, capsules or granules, breaking, accurately weighing 3-10g of sample, putting into a centrifugal tube provided with a plug, then adding 20-60mL of homemade extract, mixing, carrying out ultrasonic extraction for 2-10 minutes, carrying out centrifugal separation, then taking 1mL of supernatant, carrying out blow drying with nitrogen, and redissolving with 1mL of 50% acetonitrile aqueous solution; and (3) filtering the redissolved solution by virtue of a 0.22 microns microporous membrane, and carrying out HPLC-MS / MS (high performance liquid chromatography+mass spectroscopy+secondary mass spectroscopy detection) determination on filtrate.

Description

technical field [0001] The invention relates to the technical field of drug residue detection, in particular to a rapid detection method for illegally added hypoglycemic and antihypertensive drug residues in health care products. Background technique [0002] Health (functional) food is a category of food, which has the commonality of general food, can regulate the function of the human body, and is suitable for consumption by specific groups of people, but not for the purpose of treating diseases. The health care function of health food is gradually being accepted by the masses in today's society. Health care products currently on the market can be roughly divided into general health food, health medicine, health cosmetics, health care products, etc., while health care medicines are nutritious and food-based natural medicines, and should be used in conjunction with treatment, with usage and dosage requirements. Drugs with "healthy" batch numbers, but in order to increase m...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 叶佳明史立文许荣年叶磊海应寒松詹越城陈青俊
Owner 浙江公正检验中心有限公司
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