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UPLC-MS/MS detecting method for detecting concentration of parabens preservatives in human urine

A technology of p-hydroxybenzoic acid and propyl paraben, which is applied in the field of UPLC-MS/MS detection of the concentration of paraben preservatives in human urine, can solve the problems of large dosage, gastrointestinal discomfort, etc. Achieve the effect of high sensitivity and strong anti-interference ability

Inactive Publication Date: 2016-12-21
HARMONIA TESTING TECH TIANJIN LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Large doses of ethyl paraben can also cause gastrointestinal discomfort to the human body

Method used

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  • UPLC-MS/MS detecting method for detecting concentration of parabens preservatives in human urine
  • UPLC-MS/MS detecting method for detecting concentration of parabens preservatives in human urine
  • UPLC-MS/MS detecting method for detecting concentration of parabens preservatives in human urine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0035] Detection of the concentration of parabens in sample 1, sample 2, sample 3, sample 4, and sample 5 (the sample processing method and detection conditions are the same):

[0036] (1) Standard product treatment: Take 500uL of urine, add 50uL of standard solution, and prepare a series of solutions corresponding to the concentrations of plasticizer components in urine: 5, 10, 25, 50, 100, 250, 500ng / ml . Add 50uL of β-glucuronidase (80U / mL), shake well and seal, put in a 37°C water bath and heat for 120min. After the reaction, take 100uL of the reaction solution, add 300uL of precipitant (methanol / acetonitrile=1:1) to precipitate the protein, vortex and mix well, centrifuge at 15000rpm for 10min, and take 5uL of the supernatant for sample analysis.

[0037] (2) Standard curve creation: take the concentration of the analyte as the abscissa, and the difference between the peak area of ​​the analyte and the peak area of ​​the corresponding component of the urine sample as the...

Embodiment 2

[0052] 2.1 Method recovery experiment

[0053] Take six parts of the test solution, add equal volumes of 10, 100, 800ng / ml reference substance solutions of each component, mix well, prepare 5, 50, 400ng / ml reference substance solutions of each component, inject samples, and operate in parallel for each sample Six copies were used to calculate the recovery rate. The results are detailed in Table 5.

[0054] Table 5 recovery rate test result

[0055]

[0056]

[0057] 2.2 Method precision experiment

[0058] According to the QC sample preparation method, 5, 50, and 400 ng / ml solutions of each component were prepared, injected, and each sample was operated in parallel six times to investigate the precision of the method. The results are detailed in Table 6.

[0059] Table 6 method precision test results

[0060]

[0061]

[0062]

[0063] 2.3 Solution stability test

[0064] According to the QC sample preparation method, 5, 50, and 400 ng / ml component solutio...

Embodiment 3

[0069] The preparation and detection conditions of the lowest quantification limit (5ng / ml) concentration mixed standard and the mark line (25ng / ml) concentration mixed standard:

[0070] (1) Standard product treatment: Take 500uL of urine, add 50uL of standard solution, and prepare a series of solutions corresponding to the concentrations of plasticizer components in urine: 5, 10, 25, 50, 100, 250, 500ng / ml . Add 50uL of β-glucuronidase (80U / mL), shake well and seal, put in a 37°C water bath and heat for 120min. After the reaction, take 100uL of the reaction solution, add 300uL of precipitant (methanol / acetonitrile=1:1) to precipitate the protein, vortex and mix well, centrifuge at 15000rpm for 10min, and take 5uL of the supernatant for sample analysis.

[0071] (2) Standard curve creation: take the concentration of the analyte as the abscissa, and the difference between the peak area of ​​the analyte and the peak area of ​​the corresponding component of the urine sample as ...

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Abstract

The invention provides a UPLC-MS / MS detecting method for detecting concentration of parabens preservatives in human urine. The method includes the steps of firstly, processing samples, to be more specific, placing a to-be-detected urine sample into a test tube or a centrifugal tube, adding water with the volume being 1 / 10 times of the volume of the urine sample, adding beta-glucuronidase, shaking up and sealing, heating in water bath of 37 DEG C until complete reaction is achieved, taking a certain amount of reaction liquid, adding precipitator (methanol / acetonitrile=1:1) with the quantity being 3 times of the quantity of the reaction liquid to precipitate protein, well mixing in a vortex manner, centrifuging at 15000rpm for 10 minutes, and taking 5-10 microliters of supernate for sample analysis; secondly, injecting the sample, and performing the UPLC-MS / MS detection according to certain conditions; thirdly, calculating the concentration of the parabens preservatives in the human urine according to the peak area of the sample and the regression equations of standard curves. The UPLC-MS / MS detecting method has the advantages that the method is simple and fast, high in sensitivity, high in interference resistance and suitable for the simultaneous qualitative and quantitative detection of the preservatives in the urine, and food with excessive preservatives can be detected in the urine through metabolism.

Description

technical field [0001] The invention belongs to the field of biological analysis, in particular to a UPLC-MS / MS detection method for the concentration of p-hydroxybenzoate preservatives in human urine. Background technique [0002] Parabens, also known as parabens, are colorless crystals or crystalline powders at room temperature, including their methyl, ethyl, propyl, isopropyl, butyl, isobutyl, etc., usually In other words, with the increase of its alkyl carbon chain, its toxicity is reduced and its antibacterial effect is enhanced. Parabens have poor water solubility, and their water solubility can be improved by synthesizing their sodium salts. [0003] Methyl p-hydroxybenzoate, also known as methylparaben or methylparaben, white crystalline powder or colorless crystal, easily soluble in alcohol, ether and acetone, very slightly soluble in water, boiling point 270-280°C. It is mainly used as a bactericidal preservative in organic synthesis, food, cosmetics, and medicin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/02
CPCG01N30/02G01N2030/027
Inventor 付淑军张文怡李英李安平袁圆王文佳
Owner HARMONIA TESTING TECH TIANJIN LTD
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