Method for determining antibacterial agent triclosan in antibacterial textiles by gas chromatography-mass spectrometry

Method for determining antibacterial agent triclosan in antibacterial textiles by gas chromatography-mass spectrometry

Key words : antibacterial agent, triclosan, gas chromatography-mass spectrometry, antibacterial textile, test method

Abstract : The antibacterial agent triclosan in antibacterial textiles was extracted by ultrasonic extraction with dichloromethane as the extraction solvent. The method of gas chromatography-mass spectrometry for the detection of triclosan in antibacterial textiles was established. The extraction conditions were optimized. The method is simple, rapid and sensitive . The detection limit of triclosan is 0 under the condition of signal to noise ratio of 3 . 05 mg / L , the average recovery was 95 . 38% to 98 . 60% with a relative standard deviation of 2 . 93% to 4 . 44% . The actual sample was measured by this method, and it was found that some commercially available antibacterial textiles contained a high concentration of the antibacterial agent triclosan.

Triclosan (2 , 4 , 4 ' - trichloro -2 ' - hydroxydiphenyl ether) is a broad spectrum antibacterial agent, having a high bactericidal action, had been considered highly safe to the environment and human [1], thereby obtaining a wide range of applications [2]. In the textile industry, triclosan is usually mixed into a molten polymer to be spun, uniformly dispersed in the inside of the fiber to obtain an antibacterial fiber, and further processed into various antibacterial fabrics [ 3 ]. A variety of antibacterial fabrics containing triclosan are currently on the market for sale. However, recent research shows that triclosan has certain toxicity to aquatic organisms [ 4-5 ], and it also produces strong carcinogens during photocatalytic degradation [ 6 ]. Although it has not been reported that triclosan is toxic to mammals, countries have adopted legislation to restrict the use of triclosan. The restrictions have gradually expanded from daily chemical products and detergents to food contact materials and textiles. Norway has enacted The PoHS Directive stipulates that the triclosan content of textiles must not exceed 10 mg/kg .

At present, the detection of triclosan at home and abroad is mainly concentrated on daily chemical products and environmental samples. The determination of triclosan in textiles has not been reported in the literature. Triclosan is determined by high performance liquid chromatography (HPLC) [ 7 ], LC/MS ( 8 /MS) [ 8 ], GC/MS (GC/MS) [ 9 ], spectrophotometry [ 10 ]. Wait. When triclosan is determined by GC/MS , it is generally necessary to derivatize triclosan [ 11-12 ]. The commonly used derivatization reagents are acetic anhydride, N -methyl- N ( trimethylsilyl ) -three. Fluoroacetamide, N , O- bis ( trimethylsilyl ) -trifluoroacetamide, and the like. In this paper, acetic anhydride was used as a derivatization reagent to establish a method for the determination of triclosan in antibacterial textiles by gas chromatography-mass spectrometry. The method is simple and rapid.

1 • Experimental part

1 . 1 instruments and reagents

Instrument: GC 3800-Varian 1200 gas chromatograph - mass spectrometer (Varian Inc. U.S.), autosampler with a triple and a DB-5MS capillary column ( 30 m × 0 . 25 mm × 0 . 25 μ m); SK2510HLC ultrasonic cleaner (Shanghai Branch I. Ultrasonic Instrument Co.); 4003 Heidolph rotary evaporator (Heidolph, Germany) equipped cooling water system; nitrogen blowing instrument (Beijing Conlin Technology Co., Ltd.) ;SHZ-B water bath thermostatic oscillator ( Shanghai Yuejin Medical Instrument Factory ) .

Reagents : acetic anhydride, absolute ethanol, isopropanol, acetone, dichloromethane, n-hexane, petroleum ether, cyclohexane, sodium tetraborate are analytically pure, all provided by Guangzhou Chemical Reagent Factory ; experimental water is secondary distilled water, methanol (HPLC grade) supplied by the company Tedia; triclosan standards (purity 995 mass fraction) by the German Dr. Provided by Ehrenstorfer .

0 . Preparation of 1 mol/L sodium tetraborate aqueous solution : weigh 38 . 1 g Sodium tetraborate dissolved in double distilled water to a constant volume 1 L .

1 . 2 standard solution preparation

Weigh the standard sample of triclosan 10 . 0 mg , dissolved in methanol, dilute to 10 ml , to obtain a standard stock solution with a concentration of 1 mg/ml , and dilute to a standard solution of various concentrations with double distilled water.

1 . 3 sample preparation

For the fabric sample to be tested, take a representative part and cut it into 0 . 5 cm × 0 . 5 cm Small pieces, weighed and weighed 1 . 0 g The sample was placed in a 150 ml fryer, and 25 ml of extraction solvent was added and ultrasonically extracted at room temperature for 30 min . The extracted sample was filtered and the filtrate was transferred to a chicken heart bottle. The filtrate was rotary evaporated to near dryness, dried with nitrogen, washed with 50 ml of aqueous sodium tetraborate solution, and transferred to a 150 ml milled flask. Add 1 ml of acetic anhydride to the washing solution, shake at room temperature for 30 min at 500 r/min , add 10 ml of n-hexane, continue to shake for 30 min , then transfer to a 125 ml separatory funnel. After standing, the solution is divided. It is two layers. The upper layer solution is the organic phase and the lower layer solution is the aqueous phase. Discard the lower aqueous phase solution. The upper organic phase solution was washed 3 times with 30 ml of sodium tetraborate to remove impurities, using 0 . 2 μ m filter pore size (the filter provided by the German company Membrana) for testing after filtration. If necessary, dilute the organic phase before injecting the sample.

After the triclosan standard solution was subjected to ethylation, chromatographic analysis was carried out.

1 . 4 chromatographic conditions

Column : DB-5MS capillary column ( 30 m × 0 . 25 mm × 0 . 25 μ m) .

Column temperature : initial temperature 150 °C To 20 °C /min rose to 280 °C , constant temperature 3 . 5 min . Inlet temperature : 250 °C ; Chromatography - mass Interface Temperature: 260 °C ; ion source temperature : 200 °C ; Carrier gas: helium, purity ≥ 99. 999% volume fraction, flow rate 1 . 0 ml / min; injection volume : 1 . 0 L ; injection method : no split injection, 1 . Valve opening after 0 min ; ionization mode : electron bombardment ion source (EI); mass scanning range : 45 ~ 550 amu; full scan mode ; ionization energy : 70 eV; electron multiplier voltage : 1 . 1 kV; solvent delay : 4 . 0 min; quantitative ion m/z: 288 , 330 .

2 • Results and discussion

2 . 1 extraction reagent and extraction time selection

Triclosan is slightly soluble in water and soluble in many organic solvents. Therefore, the first choice is methanol, ethanol, isopropanol, acetone, n-hexane, cyclohexane, petroleum ether, dichloromethane, water and other common solvents. To extract triclosan in textiles. As can be seen from Table 1 , the extraction of triclosan by methylene chloride is the most efficient, followed by methanol and ethanol. Therefore, the final choice of dichloromethane is used as the extraction solvent.

8 samples were taken, with dichloromethane as the extraction solvent are ultrasonic extraction 5, 10, 15, 20, 25, 30, 35, 40 min, and found that, with the increase in extraction time, the extraction amount of triclosan gradually Increase ; when the extraction time exceeds 30 min , the extraction amount hardly increases. Therefore, the ultrasonic extraction time selected in this paper is 30 min .

2 . 2 Determination of the volume of acetic anhydride

Acetic anhydride is esterified with triclosan, and the resulting triclosan is extracted into n-hexane. At the same time, excessive acetic anhydride reduces the pH of the solution , which also has a certain effect on the extraction effect. Take 9 parts of triclosan standard solution and add 0 respectively . 2 , 0 . 5 , 1 . 0 , 1 . 5 , 2 . 0 , 2 . 5 , 3 . 0 , 3 . 5 , 4 . 0 ml of acetic anhydride was subjected to esterification, and the chromatographic peak area of ​​triclosan was determined. The results are shown in Fig. 1 . It can be seen from Fig. 1 that as the volume of acetic anhydride increases, the area of ​​the extraction peak gradually increases ; when the volume of acetic anhydride is 1 . When the concentration is 0 ml , the extraction efficiency is the highest ; when the volume of acetic anhydride is further increased, the extraction effect is decreased. Therefore, the final determined volume of acetic anhydride is 1 . 0 ml .

2 . 3 qualitative and quantitative analysis

When the sample is measured, if the detected mass peak retention time is consistent with the standard, and the relative abundance of the qualitative ion is less than 10% compared with the standard spectrum , it can be judged that the antibacterial agent trichloride is present in the sample. Health. The total ion current diagram of the derivatized product of the triclosan standard is shown in Fig. 2 , and the quantitative ion m/z is 288 , 330 .

2 . 4 linear relationship and detection limit

Under the experimental conditions determined by the triclosan determination method herein, different concentrations of triclosan standard solution were determined, and the results showed that at 0 . 1 ~ 80 . In the range of 0 mg/L , the concentration of triclosan has a good linear relationship with the instrument response. The linear equation is :

The detection limit of the method is determined by adding a certain concentration of triclosan standard solution to the textile containing no triclosan, and the detection limit is determined under the condition of S/N ( signal-to-noise ratio )=3 . Is 0 . 05 mg/L .

2 . 5 precision and recovery experiments

Add three concentration levels of triclosan standard solution to the textile containing no triclosan, press 1 . The procedure in Section 3 is processed to determine the recovery rate of triclosan. The results are shown in Table 2 . It can be seen from Table 2 that the determination method of triclosan has high recovery rate and good precision. Under the three added concentration levels, the relative standard deviation (RSD) of the precision test is less than 5% .

2 . 6 actual sample test

Commercially available antibacterial textiles were tested and the antibacterial agent triclosan was detected in some samples. Figure 3 is a total ion chromatogram of a military green woven polyester dyed cloth. The antibacterial agent triclosan was detected in the sample, and its content was 12 815 . 7 mg/kg .

3 • Conclusion

Using dichloromethane as the extraction solvent, the antibacterial agent triclosan in the antibacterial textile was ultrasonically extracted . The extract was derivatized and determined by gas chromatography-mass spectrometry. A gas chromatography-mass spectrometry was established. A method for the antibacterial agent triclosan in antibacterial textiles. The method has high recovery rate of triclosan and high precision, and the detection limit is 0 . 05 mg/L . The commercially available antimicrobial textile was measured by this method, and it was found that some commercially available antimicrobial textiles contained a high concentration of the antibacterial agent triclosan.

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