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A method for determining illegally added compounds in health food

A technology for illegal addition and health food, applied in measuring devices, instruments, scientific instruments, etc., can solve the problems of complicated operation of mobile phase, complicated and difficult extraction of solution, etc.

Active Publication Date: 2021-09-24
徐敦明
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since methanol is easily soluble in water, this method cannot achieve the separation of active ingredients in liquid medicines, and cannot detect oral liquid health foods
In terms of chromatographic conditions, the gradient elution of formic acid aqueous solution and acetonitrile as mobile phase will cause adverse effects such as complicated operation of mobile phase, and only 6 kinds of illegal additives can be determined.
[0005] Patent application CN108061777A discloses a rapid detection method for 34 kinds of illegally added drug residues in weight-loss health food. The target object is extracted with methanol, acetone and octanol polyoxyethylene ether. The above problems also exist, and acetone will make the extraction solution complicated. And lead to serious adverse effects of matrix interference, octanol polyoxyethylene ether is a relatively special organic reagent that is not suitable for popularization and application, so the extraction solution formed by mixing methanol, acetone and octanol polyoxyethylene ether is too complicated to adapt to many matrices

Method used

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  • A method for determining illegally added compounds in health food
  • A method for determining illegally added compounds in health food
  • A method for determining illegally added compounds in health food

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 121

[0070] Example 1 establishes the basis for qualitative judgment with standard samples of 21 illegally added compounds

[0071] Standard products: ephedrine, sibutramine, N,N-bisdesmethylsibutramine, N-monodemethylsibutramine, fenfluramine, phenformin, piroglitazone, Glipizide, repaglinide, gliclazide, glyburide, tolbutamide, glimepiride, gliquidone, glibouride, clonidine, reserpine, deshydroxylova Statins, mevastatin, lovastatin, and simvastatin were directly injected into the liquid chromatography-mass spectrometer. Mass spectrometry conditions: electrospray ionization ion source; scanning mode is positive ion scanning; detection mode is MRM mode; desolvation gas flow rate is 900L / H; desolvation gas temperature is 650°C. The standards were analyzed by primary mass spectrometry to obtain their parent ions. Scan the standard by MS / MS to obtain the product ion information of the substance, and determine the quantitative and qualitative ion pairs of the target compound. By opt...

Embodiment 2

[0077] The optimization of embodiment 2 chromatographic conditions

[0078] The response of each substance was tested when methanol-water and ammonium acetate aqueous solution-methanol were used as the mobile phase. The experiment found that when the methanol-water system was used as the mobile phase, the response of compounds such as lipid-lowering compounds was significantly enhanced, and the compounds were separated. The effect is better. In addition, adding 7-12mmol / L ammonium acetate to water can obviously improve the peak shape. Preferably 10mmol / L ammonium acetate-methanol system is used as mobile phase, and the analysis time of 21 kinds of compounds is shorter, and the separation is good, and the response is high.

Embodiment 3

[0079] The optimization of embodiment 3 purification method

[0080] For the functional groups present in the structural formulas of 21 compounds, such as quaternary ammonium ions and benzene rings, the purification effect of QuECHERS (900mg Mg2SO4, 150mg PSA, 15mg GCB), PAX SPE, HLB SPE on standard samples was investigated experimentally. The results showed that QuECHERS And the recovery rate of PAX to some compounds is not ideal, but the recovery rate of the target compound is better when the HLB column is used, and HLB is finally selected as the purification column.

[0081] The establishment of the target compound eluting curve: the aqueous solutions of 21 target compounds were loaded, and then respectively washed with 0%, 5%, 10%, 20%, 30%, 40%, 50%, 60%, 70%, 80% , 90%, and 100% methanol aqueous solution were eluted, and the eluent was collected for measurement on the machine. The concentration of methanol water was used as the abscissa, and the recovery rate was used as...

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Abstract

The invention relates to a method for determining illegally added compounds in health food, comprising step 1: directly injecting standard samples of illegally added compounds into a mass spectrometer to obtain mass spectrometer parameters of target compounds as a basis for qualitative judgment, and drawing a standard curve, As the basis for quantitative calculation; Step 2: Weigh the weight of the sample to be tested, after ultrasonic extraction with acetonitrile, HLB solid-phase extraction column purification, to obtain the sample solution; Step 3: Send the sample solution to liquid chromatography mass spectrometry Instrument for qualitative and quantitative judgment; wherein the liquid chromatography conditions are: the chromatographic column is a C18 chromatographic column; the mobile phase is ammonium acetate aqueous solution and methanol. The method provided by the invention can simultaneously determine 21 kinds of illegally added compounds in health food, including health food for weight loss, lipid-lowering, blood pressure, and sugar. The food form is not limited to oral liquid, granules, tablets, hard capsules or Softgels.

Description

technical field [0001] The invention relates to a drug detection method, in particular to a method for determining illegally added compounds in health food. Background technique [0002] At present, the detection methods for illegally added drugs in weight loss, lipid-lowering, sugar-lowering, and blood-pressure-lowering health foods mainly include liquid chromatography, liquid chromatography-mass spectrometry, Raman spectroscopy, and thin-layer chromatography. Among them, ultra-high performance liquid chromatography tandem mass spectrometry has been widely used in the qualitative and quantitative analysis of illegally added drugs in health food because of its high selectivity and high sensitivity. The difficulty of using ultra-high performance liquid chromatography tandem mass spectrometry is that a set of detection methods is often a complete system, and the steps before and after are closely related. For example, extracts obtained from different extraction solvents requir...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): G01N30/88
Inventor 徐敦明赖国银黄蓬英伊雄海罗超陈燕张志刚
Owner 徐敦明