Recently, the CFDA has released a variety of detection methods for banned substances such as thioglycolic acid, dioxane, lidocaine, mercury, and desloratadine in cosmetics, involving various detection methods such as GC-MS and ICP-MS. The technical requirements for the detection of substances in cosmetics are prohibited, and the quality and safety of cosmetics are improved. The method for detecting prohibited substances has been reviewed and approved by the Expert Committee on Cosmetic Standards.
Skyray Instruments has always been committed to providing customers with the most complete solutions. For the announced testing project, Tianrui Instrument GC-MS 6800 can be used for the detection of dioxane and volatile organic solvents in cosmetics.
1. Introduction to the instrument
GC-MS 6800 is a cost-effective gas chromatography mass spectrometer designed by Tianrui Instruments. It has complete independent intellectual property rights and possesses a number of patented technologies. It can be widely used in environmental protection, electronic appliances, medicine, petrochemicals, Detection of harmful substances in many industries such as food safety and textile leather.
Figure 1. Appearance of GC-MS 6800 Gas Chromatography Mass Spectrometer
2. Experimental part
2.1 Detection of dioxane in cosmetics
2.1.1 Dioxane Introduction Dioxane, also known as 1,4-dioxane, is a colorless liquid found in many media in nature. The human body contacts dioxane through the skin, respiratory tract and digestive tract. Dioxane is exposed to exposure to occupational exposure, breathing to the air, drinking water or eating foods that may contain dioxane, as well as washing products, cosmetics, topical medicines, and agricultural products that may contain dioxane. Dioxane is a banned substance in cosmetics. Dioxane enters the body by inhalation, ingestion, and percutaneous absorption. It has anesthesia and stimulating effects and has an accumulation in the body.
2.1.2 Main instruments, consumables and reagents
GC-MS 6800 Gas Chromatography Mass Spectrometer + Headspace Autosampler (Jiangsu Tianrui Instrument Co., Ltd.),
Electronic balance (one thousandth of precision), ultrasonic cleaning machine, sodium chloride, dioxane standard solution, glassware used in other laboratories, etc.
2.1.3 Detection principle After the sample was heated and extracted in the headspace bottle, it was determined by gas chromatography-mass spectrometry, and the retention time and characteristic ion relative abundance ratio were used for qualitative determination. The ion monitoring mode was selected for measurement and external standard method was used for quantification.
2.1.4 Instrument test conditions Headspace injection conditions Vaporization chamber temperature: 70 ° C; Dosing tube temperature: 150 ° C; Transmission line temperature: 200 ° C; Oscillation: Oscillation;
Vapor-liquid equilibrium time: 40min; injection time: 1min;
GC-MS 6800 test condition chromatography column: DB-5MS, 30m × 0.25mm × 0.25um;
Oven temperature programming conditions: 40 ° C (8 min) 10 ° C / min 220 ° C (10 min);
Inlet temperature: 220 ° C;
Chromatography-mass interface temperature: 220 ° C;
Carrier gas: helium, purity ≥99.999%, flow rate 1.0mL/min;
Ionization mode: EI; ionization energy: 70eV;
Injection method: split injection, split ratio 1..1; injection volume: 1.0mL;
Determination method: TIC (FULL SCAN) qualitative, SIM mode quantitative.
Figure 2. Total ion chromatogram (TIC) of dioxane
Figure 3. Mass spectrum of dioxane standard solution
2.2 Detection of volatile organic compounds in cosmetics
2.2.1 Introduction to Volatile Organic Compounds Volatile organic compounds, the English name is Volatile Organic Compound (VOC), defined by WHO (World Health Organization) as boiling point at 50-250 ° C, saturated vapor pressure at room temperature over 133.32 MPa, at room temperature A type of organic matter in the form of steam in the air, mainly containing alkanes, aromatic hydrocarbons, halogenated hydrocarbons, esters, aldehydes, ketones and the like. Its main sources are industrial waste gas generated by fuel combustion and transportation, automobile exhaust, photochemical pollution, etc., and the release of interior decoration materials. VOC harms the human body mainly by irritating the eyes and respiratory tract, causing allergies, headaches, sore throats, and fatigue.
2.2.2 Main instruments, equipment, consumables and reagents
GC-MS 6800 Gas Chromatography Mass Spectrometer + Headspace Autosampler (Jiangsu Tianrui Instrument Co., Ltd.),
Electronic balance (one thousandth of a thousandth, one thousandth), ultrasonic cleaner, vortex mixer,
Methanol (chromatographically pure), sodium chloride (excellent grade), volatile organic standard solution, glassware used in other laboratories, etc.
2.2.3 Test principle This method uses headspace injection, disperse the sample with water (the fat-soluble sample is added with appropriate amount of methanol), analyze it by gas chromatography-mass spectrometer, and characterize the retention time and characteristic ion abundance ratio to select ion monitoring. The mode is tested and the external standard method is used for quantification.
2.2.4 Instrument test conditions Headspace reference conditions Equilibrium temperature: 60 ° C, injection temperature: 100 ° C, transmission line temperature: 120 ° C, equilibration time: 30 min, loop: 1 mL;
GC-MS 6800 test condition chromatography column: DB-624, 60 m × 0.25 mm × 1.4 μm; flow rate: 1.0 mL / min;
Inlet temperature: 150 ° C, injection method: split injection, split ratio 50:1
Temperature programmed: 30 ° C (10 min) 5 ° C / min 100 ° C 30 ° C / min 220 ° C (5 min);
Electron bombardment source, collision energy 70eV; ion source temperature 230°C; temperament interface temperature: 220°C; full scan mode (FULL SCAN) and selective ion monitoring (SIM) mode.
Figure 4. Selected ion monitoring mode diagrams for 54 volatile organic compounds (SIM)
1, 1,1-dichloroethylene 2, dichloromethane 3, trans 1,2-dichloroethylene 4,1,1-dichloroethane 5, cis 1,2-dichloroethylene/2,2 -dichloropropane 6, bromochloromethane 7, 8, 1,1,1-trichloroethane 9, 1,1-dichloropropene / carbon tetrachloride 10, benzene / 1,2-dichloroethane 11 , trichloroethylene 12, 1,2-dichloropropane 13, dibromomethane 14, monobromodichloromethane 15, cis 1,3-dichloropropene 16, toluene 17, trans 1,3-dichloropropene 18 1,1,2-trichloroethane 19, tetrachloroethylene 20, 1,3-dichloropropane 21, dibromochloromethane 22, 1,2-dibromoethane 23, chlorobenzene 24, 1,1 1,2-tetrachloroethane 25, ethylbenzene 26, m-p-xylene 27, o-xylene 28, styrene 29, bromoform 30, cumene 31, bromobenzene / 1,1,2,2 -tetrachloroethane 32, 1,2,3-trichloropropane 33, n-propylbenzene 34, 2-chlorotoluene 35, 1,3,5-trimethylbenzene 36, 4-chlorotoluene 37, tert-butyl Benzene 38, 1,2,4-trimethylbenzene 39, sec-butylbenzene 40, 1,4-dichlorobenzene 41, 4-isopropyltoluene 42, 1,3-dichlorobenzene 43, n-butyl Benzene 44,1,2-dichlorobenzene 45, 1,2-dibromo-3-chloromethane 46, 1,2,4-trichlorobenzene 47, hexachlorobutadiene 48, naphthalene 49, 1,2, 3-trichlorobenzene
summary
The GC-MS 6800 Gas Chromatography Mass Spectrometer is equipped with a headspace autosampler to effectively monitor the content of dioxane and volatile organic compounds in cosmetics to meet the monitoring needs of the cosmetics industry.
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