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Method for detecting residue of 22 illegally-added nerve-calming drugs in health product

A technology for illegal addition and detection methods, applied in the direction of measuring devices, instruments, scientific instruments, etc., can solve the problems of cumbersome operation, single processing method, long time consumption, etc., to achieve high dissolution efficiency, improve detection efficiency, and shorten the effect of time

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

However, the operation is cumbersome and time-consuming, and the sample processing method for different matrices is single, and the detection interference is relatively large; in addition, the detection method for the simultaneous determination of these 22 sedative and tranquilizing chemicals has not yet been established

Method used

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  • Method for detecting residue of 22 illegally-added nerve-calming drugs in health product
  • Method for detecting residue of 22 illegally-added nerve-calming drugs in health product
  • Method for detecting residue of 22 illegally-added nerve-calming drugs in health product

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a drug residue detection technology and aims at providing a method for detecting residue of 22 illegally-added nerve-calming drugs in a health 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 22 illegally-added nerve-calming drugs in the health product comprises the following steps: (1) preparing homemade extract, namely refluxing a mixture of methyl alcohol, ethyl acetate and capryl 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, thenadding 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% methanol aqueous solution; and (3) filtering the redissolved solution by virtue of a 0.22 micron 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 a drug residue detection technology, in particular to a rapid detection method for illegally added calming drug residues in health products. Background technique [0002] With the changes in people's life rhythm in recent years, sleep problems caused by various pressures such as life, study, and work have become more and more serious, and the number of people with insomnia has increased. Some people need to rely on sedative and tranquilizing drugs to maintain normal sleep and life. Most patients will choose to buy traditional Chinese medicine and health care products in the market to relieve symptoms, thinking that their effects are milder and have fewer adverse reactions. Therefore, some unscrupulous merchants illegally add sedative and hypnotic chemical drugs in traditional Chinese medicine preparations and health products in order to make huge profits and enhance their publicity effects, so as to enhance the efficacy of the ...

Claims

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Application Information

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IPC IPC(8): G01N30/02G01N30/06
CPCG01N30/02G01N30/06
Inventor 钟世欢史立文许荣年叶磊海张海萍陈青俊顾秀英
Owner 浙江公正检验中心有限公司
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