Key words
TRACE GC 1310; hydrogen flame ionization detector; preservative; GB/T 24800.11-2009
aims
With reference to GB/T 24800.11-2009, a gas chromatography method with simple operation, simple sensitivity and accurate analysis was established for the analysis of benzyl alcohol in cosmetics.
introduction
Benzyl alcohol, also known as benzyl alcohol, is an aromatic alcohol used as an aromatic component, preservative, solvent and viscosity reducer in various cosmetics. It is a new preservative in recent years. Due to the strong toxicity of benzyl alcohol, it has been restricted by some countries in some aspects. China has also made clear provisions for benzyl alcohol. In the "Hygienic Standard for Cosmetics (2007)", benzyl alcohol is used as a restricted substance, and the content should not exceed 1% [1] . China has also issued the corresponding test standard GB/T24800.11-2009 "Preparation of benzophenone in cosmetics, gas chromatography" [2] .
This article refers to GB/T24800.11-2009 "Preparation of Benzyl Alcohol in Cosmetics by Gas Chromatography", using Thermo Scientific TRACEGC1310 Gas Chromatography to analyze benzyl alcohol in various cosmetics. The method is sensitive, accurate, simple and feasible. Easy to promote and apply.
instrument
Thermo Scientific TM TRACE GC 1310 GC, including:
- SSL inlet;
- FID detector;
- AS1310 105-position liquid autosampler
- Thermo Scientific TM Dionex TM Chromeleon TM Chromatography Data System software, version 7.2 SR1
Reagents and standards
The benzyl alcohol standard was purchased from Aladdin Reagent (Shanghai) Co., Ltd.; absolute ethanol, HPLC grade (Fisher Scientific P/N A407-1).
Sample preparation
Refer to Section 5.2.1 of GB/T24800.11-2009: Weigh about 0.5g (accurate to 0.01g) of the sample into a 10mL volumetric flask, add 5mL of absolute ethanol, ultrasonically extract for 20min, and dilute to the mark with ethanol. After mixing, transfer to a 10 mL centrifuge tube and centrifuge at 3000 r/min for 10 min. The supernatant was passed through a 0.45 μm filter and analyzed by GC.
Experimental condition
Chromatographic conditions
Column: TG-5MS (30 m × 0.25 mm × 0.25 μm, P / N: 26098-1420;
Column temperature: 100 ° C (3 min), 10 ° C / min to 220 ° C (0 min), 40 ° C / min to 300 ° C (5 min); split injection, split ratio of 5:1;
Inlet temperature: 250 ° C; Carrier gas: Nitrogen (99.999%), constant flow mode, 1.0 mL/min. FID detector temperature: 300 ° C; hydrogen flow rate: 35 mL / min, air flow rate: 350 mL / min, makeup gas: 40 mL / min.
Chromatogram
Methodological data
Appropriate standards were prepared and configured as 0.5, 1.0, 2.0, 5.0, 10.0 and 20.0 mg/L standard curve working solutions. The above methods were used to analyze the linearity of benzyl alcohol in the linear range of 0.5-20.0 mg/L. The experimental results show that the linear relationship of benzyl alcohol is good, the linear correlation coefficient is 0.9997 (Fig. 3), the detection limit is 0.15 mg/L, and the limit of quantification is 0.50 mg/L.
Actual sample testing and standard recovery
A total of 6 samples of facial cleanser, lotion, lotion and lipstick were purchased in the supermarket and tested by this method. The experimental results showed that the tested benzyl alcohol was not detected in any of the six samples (see Figure 3 for chromatogram).
At the same time, the emulsion samples were taken in this experiment, and three different levels of spiked recovery experiments were carried out. The spiked concentrations were 0.5, 1.0 and 10.0 mg/L, and the recovery of benzyl alcohol was investigated. The experimental results show that the three levels of spiked recovery are 105.2%, 95.6% and 96.3%, respectively, in line with the requirements of daily analytical testing (Figure 3). A parallel injection of 0.5 mg/L standard solution for 6 needles showed a peak RSD of 2.35% and a retention time RSD of 0.04%.
to sum up
The method was carried out using Thermo Fisher Scientific's new generation TRACE 1310 GC, which fully meets the requirements of detection sensitivity and precision. At the same time, the pretreatment of the method is simple and rapid, the recovery rate of the standard addition is high, the detection sensitivity of the instrument is high, and the linear range is good.
references
[1] Ministry of Health of the People's Republic of China. "Hygienic Standards for Cosmetics" [S], 2007.01.
[2] National Standard of the People's Republic of China. GB/T 24800.11-2009, Determination of Preservative Benzyl Alcohol in Cosmetics by Gas Chromatography [S].
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