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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

Active Publication Date: 2018-05-22
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

However, some unscrupulous merchants directly add some illegally used drugs to health food to achieve specific drug effects, such as weight loss drugs indapamide, bisacodyl, fenofibrate, etc.
The abuse of these drugs will have a serious impact on people's health. Therefore, it is of social significance to establish a simple, fast, sensitive and adaptable method for the determination of illegally added drug residues in weight-loss health foods.
[0003] According to the existing methods for detecting the residues of weight-loss drugs illegally added in health products, there are only the State Food and Drug Administration Drug Inspection Supplementary Inspection Methods and Inspection Items Approval Document 2006004, and the State Food and Drug Administration Drug Inspection Supplementary Inspection Methods and Inspection Project approval document 2012005, State Food and Drug Administration Announcement on Food Supplement Inspection Methods (2017 No. 24 Attachment), there is no formal national standard inspection method, and the existing methods have poor matrix adaptability and insufficient coverage of drug types The problem

Method used

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  • Method for detecting residual quantity of 34 illegally-added medicines in weight-losing health food
  • Method for detecting residual quantity of 34 illegally-added medicines in weight-losing health food
  • Method for detecting residual quantity of 34 illegally-added medicines in weight-losing health food

Examples

Experimental program
Comparison scheme
Effect test

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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PUM

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Abstract

The invention relates to the technical field of medicine residue detection. An objective is to provide a method for fast detecting the residual quantity of 34 illegally-added medicines in a weight-losing health food. The method is fast and accurate, and is high in sensitivity and wide in application range. According to the technical scheme, the method comprises: 1) preparing a self-made extractedliquid, which comprises refluxing a mixture of methanol, acetone and octanol polyoxyethylene ether at 60-65 DEG C for 30 min and performing cooling for later use; 2) taking health product tablets, capsules or particles, performing pulverization, accurately weighing 3-10 g of the sample, putting the sample in a centrifuge tube provided with a plug, adding 20-60 mL of a self-made extracted liquid, performing mixing in a vortex oscillator, performing supersonic wave extraction for 2-10 min, performing centrifugation, taking 1 mL of the supernatant out, blow-drying the supernatant, and redissolving the obtained product with 2 mL of 50% of an acetonitrile aqueous solution; and 3) filtering the redissolved solution via a filter membrane with the micropore size being 0.22 mum, and measuring the filtrate via HPLC-MS / MS (that is high performance liquid chromatography and mass spectrum and secondary mass spectrum).

Description

technical field [0001] The invention relates to the technical field of drug residue detection, in particular to a rapid detection method for 34 kinds of illegally added drug residues in weight loss health food. 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. With the improvement of people's living standards, the generalization and rejuvenation of obesity have plagued some people, and the market for weight-loss and lipid-lowering health foods has become increasingly broad. However, some unscrupulous merchants directly add some illegally used drugs to health food to achieve specific drug effects, such as weight-loss drugs indapamide, bisacodyl, and fenofibrate, in order to achieve the purpose of rapid onset of effect. The abuse of these drugs will have a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
CPCG01N30/88
Inventor 王京许荣年史立文杨琳裘钧陶何斌陈青俊
Owner 浙江公正检验中心有限公司
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