Method for measuring content of wood preservatives of wooden products for children

A technology of wood preservative and determination method, which is applied in the field of determination of wood preservative content in wooden children's products, and achieves the effects of good selectivity and sensitivity, accurate quantitative results, good selectivity and sensitivity

Inactive Publication Date: 2014-01-22
CHINESE ACAD OF INSPECTION & QUARANTINE
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report on the simultaneous detection of wood preservatives in wooden children's products by gas chromatography-tandem mass spectrometry at home and abroad

Method used

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  • Method for measuring content of wood preservatives of wooden products for children
  • Method for measuring content of wood preservatives of wooden products for children
  • Method for measuring content of wood preservatives of wooden products for children

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] A method for determining the content of wood preservatives in wooden children's products, comprising the steps of:

[0031] 1. Instruments and reagents

[0032] 7890A Gas Chromatograph: Agilent Company of the United States; Quattro Micro Triple Quadrupole Mass Spectrometer: Waters Company of the United States, with EI source; Solid Phase Extraction Device: Supelco Company of the United States; NVC-2000 Rotary Evaporator: Eyela Company of Japan; P300H Ultrasonic Cleaner : Elma Company of Germany; SM2000 Cutting Mill: Retsch Company of Germany; Centrifuge: Hitachi Company of Japan; Oasis HLB solid-phase extraction column (6mL, 200mg): Waters Company of the United States.

[0033] Standard: 2,4,5-trichlorophenol, 2,4,6-trichlorophenol, 2,3,4-trichlorophenol, 2,3,4,6-tetrachlorophenol, lindane, cypermethrin, cyfluthrin , deltamethrin were purchased from Accustomard Company, purity ≥ 98%; pentachlorophenol and 2,4 dichlorophenol were purchased from Dr.Ehrenstorfer Company,...

Embodiment 23

[0050] The impact of embodiment 23 different modes on detection effect

[0051] We use the Scan mode, SIM mode (selected ion scanning mode) and MRM mode of the triple quadrupole mass spectrometer to measure a certain actual wooden toy sample (positive samples detected during the detection of actual samples, without any standard or internal standard substance addition), the results are shown in figure 2 . From the chromatogram in Scan mode, it can be seen that the composition of the wood sample is complex. When single-stage mass spectrometry SIM mode is used, some substances, especially cyfluthrin (label 8) and cypermethrin (label 9) with isomers are still affected by matrix interference. On the one hand, it cannot provide enough selectivity, which may cause qualitative problems In the case of "false positive" or "difficult to quantify", on the one hand, it cannot provide sufficient sensitivity. When the MRM mode is used, the matrix interference is significantly improved, a...

Embodiment 3

[0052] The optimization of embodiment 3 pretreatment conditions

[0053] 1. Selection of extraction solvent

[0054] Taking the absolute recovery rate of each substance in the positive sample as an indicator, the extraction effects of methanol, methanol / glacial acetic acid (9:1, v / v), ethyl acetate, and acetonitrile on wood preservatives were investigated. , 2g of wood positive samples containing 10 wood preservatives (5mg / kg, equivalent to 1mg / L on the machine) were ultrasonically extracted with 4 kinds of extracts, and concentrated, derivatized, solid-phase extracted and tested under the same conditions. machine measurement. Compared with the standard solution, the recovery rate obtained is shown in image 3 . The results showed that the extraction effects of the four solvents were significantly different, among which the extraction effect of ethyl acetate was the worst (recovery rate 74%), and the repeatability is relatively good (RSD≤12.4%, n=4), so methanol is selected...

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Abstract

The invention provides a method for measuring the content of wood preservatives of wooden products for children. The method comprises the following steps: crushing a sample to be measured, performing ultrasonic extraction by using methanol, filtering, adding an interior label working solution into the filtrate, centrifuging, filtering the supernate by using a filtering membrane, and performing spin-steaming concentration; and adding a potassium carbonate solution into the concentrated liquid, shaking uniformly, adding acetic anhydride, performing derivatization, oscillating while deflating and allowing the derivatized concentrated liquid to pass through an Oasis hydrophile lipophile balance (HLB) solid phase extraction column; sequentially leaching by using deionized water, pumping all the water by using a vacuum pump and eluting by using ethyl acetate to obtain eluent; adding a proper amount of anhydrous sodium sulfate into the eluent and drying; and performing vortical oscillation and measuring by a gas chromatography-tandem mass spectrum method. The invention establishes the method for measuring the content of 10 wood preservatives of the wooden products for children based on solid phase extraction-gas chromatography-tandem mass spectrum, which has excellent selectivity and sensitivity on detection of target objects of wood samples with complex matrix.

Description

technical field [0001] The invention relates to a method for determining the content of preservatives, in particular to a method for determining the content of wood preservatives in wooden children's products. Background technique [0002] Wooden children's products are very common in daily life, such as wooden children's furniture such as cribs, wooden toys, wooden children's tableware, etc., almost every child will come into contact with them. Whether wooden children's products are safe is closely related to children's health . At present, many manufacturers claim that their products are "made of pure natural logs", "healthy, environmentally friendly and non-toxic paint", etc., giving consumers a healthy and environmentally friendly impression. However, "logs" and "no paint" do not mean absolute environmental protection. Wood raw materials and finished products are generally treated with preservatives, and some wood preservatives are highly toxic, such as chlorophenol com...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/88
Inventor 吕庆李文涛李海玉李丕张庆白桦
Owner CHINESE ACAD OF INSPECTION & QUARANTINE
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