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Microextraction method for detecting triclosan and methyl triclosan

An extraction and methyl imidium technology, which is applied in the field of fungicide detection, can solve the problems of long time consumption, high cost, and environmental protection, and achieve the effects of simple operation, mature synthesis conditions, and improved recovery rate

Inactive Publication Date: 2017-05-31
WENZHOU MEDICAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a micro-extraction method for detecting triclosan TCS and methyltriclosan MTCS, aiming to solve the problems of time-consuming, high cost and not environmental protection in existing sample pretreatment methods

Method used

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  • Microextraction method for detecting triclosan and methyl triclosan
  • Microextraction method for detecting triclosan and methyl triclosan
  • Microextraction method for detecting triclosan and methyl triclosan

Examples

Experimental program
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Effect test

Embodiment 1

[0044] Embodiment 1: [C 4 Synthesis of MIM][NPA]

[0045] Step 1: Weigh 4g (48.7mmol) of N-methylimidazole into a single-necked flask, and then weigh 6.68g (72.2mmol) of 1-chloromethane (about 1.1 to 1.5 times the molar amount of N-methylimidazole) , slowly drop into a single-necked flask, after the dropwise addition, reflux reaction at 80°C for 24h, monitor the reaction by thin-layer chromatography, after the reaction is complete, cool the liquid in the system, evaporate excess 1-chloromethane to obtain a white solid , the yield was 90%. Step 2: Weigh 1.8g NaOH (45mmol) in a beaker (slightly excess NaOH), dissolve it with a very small amount of water, then weigh 7.53g (43.8mmol) of 1-naphthoic acid in a single-necked flask, add the completely dissolved NaOH In the system, react at 80°C for 24 hours to obtain a yellow solution, which is monitored by pointing a plate. After the reaction is completed, part of the water is evaporated, and the remaining solution is used for the ...

Embodiment 2

[0046] Embodiment 2: the detection of TCS and MTCS in the blood sample

[0047] Blood pre-treatment: Add 1mL healthy volunteer serum to a 10mL centrifuge tube, then add 4mL acetonitrile to shake for 2min, then place in a water bath at 85°C for 15min, cool and centrifuge at 5000rpm for 15min, and filter the supernatant after centrifugation (0.45 μm filter membrane), centrifuged at 10000 rpm for 5 min, and the supernatant was taken as the actual sample. Follow-up "all ionic liquid microextraction" operating procedures are as follows image 3 .

[0048] HPLC detection conditions: the mobile phase is acetonitrile (A), methanol (B) and ultrapure water (C) at a flow rate of 1.5 mL / min for binary gradient elution. The gradient elution program was as follows: 0 min, 75% acetonitrile; 3 min, 65% acetonitrile; 5 min, 50% acetonitrile; 7 min, 80% acetonitrile and 8-14 min, 70% acetonitrile, with a total run time of 8 min. The injection volume was 20 μL, the detection wavelength was 28...

Embodiment 3

[0049] Example 3: TCS and MTCS detection in urine samples

[0050] Urine pre-treatment: Add 3mL of healthy volunteer urine into a 10mL centrifuge tube, then centrifuge at 4000rpm for 10min, then filter the supernatant (0.22μm filter membrane), and take the supernatant as the actual processed sample.

[0051] HPLC detection conditions: the mobile phase is acetonitrile (A), methanol (B) and ultrapure water (C) at a flow rate of 1.5 mL / min for binary gradient elution. The gradient elution program was as follows: 0 min, 75% acetonitrile; 3 min, 65% acetonitrile; 5 min, 50% acetonitrile; 7 min 80% acetonitrile and 8-14 min 70% acetonitrile. The total run time was 8 min. The injection volume was 20 μL, the detection wavelength was 280 nm, the column temperature was 30° C., and the injection volume was 20 μL. Chromatographic peaks of TCS and MTCS in urine samples Figure 4 .

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Abstract

The invention discloses a microextraction method for detecting triclosan and methyl triclosan. An ionic liquid is imidazole naphthoates, has the characteristics of strong acidity, slight water solubility, fluorescence sensitizing effect on weak fluorescence compound and the like, and can be mixed with the traditional ionic liquid [C4MIM]BF4 to serve as a dispersing agent in the microextraction process. The ionic liquid is synthesized by the steps of enabling 1-chloromethane and N-methylimidazole to react, wherein the mole ratio of 1-chloromethane to N-methylimidazole is 1.1-1.5; enabling a reaction product to react with 1-naphthoic acid. The microextraction method disclosed by the invention has the advantages that the nonpolar environment of an extraction agent is promoted; the volume of a precipitated phase is increased; the recovery rates of TCS and MTCS are increased by 10-20%; the pH adjusting step in the microextraction process is avoided; the recovery rates in mediums such as blood plasma, urine samples, eggs, milks and the like can reach 98.6-106.1%; the minimum detection limit is as low as 0.12-0.66 [mu]g / L.

Description

technical field [0001] The invention belongs to the technical field of bactericide detection, in particular to a micro-extraction method for detecting triclosan and methyltriclosan. Background technique [0002] At present, 2,4,4'-trichloro-2'-hydroxydiphenyl ether (triclosan, TCS) is a broad-spectrum fungicide, which can be widely used in personal care products and household cleaners such as toothpaste, Shampoo, hand sanitizer, etc. Due to excessive abuse, TCS has become a ubiquitous contaminant in many matrices, including water samples, biological fluids, and various types of food. A large number of studies have shown that: TCS can be converted into 2,8-dichlorodibenzo-p-dioxin (2,8-DCDD) under light conditions, which is recognized as a toxic carcinogen in the world. Methyltriclosan (MTCS) is the methylation product of TCS, compared with TCS, its log Kow The value is 5.4, while the log of TCS Kow The value is 4.8, so MTCS has higher lipophilicity so that it can accumul...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N30/06
CPCG01N30/06G01N2030/062
Inventor 王学东王慧曲晋刚王慧利
Owner WENZHOU MEDICAL UNIV
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