CN104502509B - A kind of method measuring phenyl three (trimethylsiloxane group) silane in Food Contact silastic material - Google Patents
A kind of method measuring phenyl three (trimethylsiloxane group) silane in Food Contact silastic material Download PDFInfo
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- CN104502509B CN104502509B CN201410842189.9A CN201410842189A CN104502509B CN 104502509 B CN104502509 B CN 104502509B CN 201410842189 A CN201410842189 A CN 201410842189A CN 104502509 B CN104502509 B CN 104502509B
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Abstract
The invention belongs to technical field of analytical chemistry, a kind of specifically method measuring phenyl three (trimethylsiloxane group) silane in Food Contact silastic material, its determination step is, 1) and sample preparation: testing sample is cut into the small cubes being not more than 2 × 2 × 2 millimeters; 2) sample extraction: take a certain amount of sample in ml headspace bottle, add acetone, place a period of time after covering tightly bottle cap, then ultrasonic extraction at a certain temperature, crosses organic phase filter membrane by extract; 3) sample test: adopt gas chromatograph-mass spectrometer determination step 2) content of phenyl three (trimethylsiloxane group) silane in gained extract.Assay method sampling amount of the present invention is few, and pre-treatment is simple to operate, and test fast, and can realize the Accurate Determining of phenyl three (trimethylsiloxane group) silane in Food Contact silastic material, does is detecting of the method limited to 40? mg/kg.
Description
[technical field]
The invention belongs to technical field of analytical chemistry, specifically a kind of method measuring phenyl three (trimethylsiloxane group) silane in Food Contact silastic material.
[background technology]
Extensively elastomeric material is adopted in modern food contact material, these materials expectations can with Food Contact or with Food Contact, as rubber nipple, pressure cooker gasket, rubber packing sheet for food container and packing ring, aluminium water bottle for carrying on the back rubber sheet gasketing, inhale defeated food hose, rubber seal etc.Because these materials are in the process contacted with food, in material, some objectionable constituent may discharge or move in food, so there is strict requirement various countries for food contact material, and has put into effect some corresponding laws and regulations.These food contact materials need detection adjuvant wherein, decomposition or catabolite, monomer residue thing, also have the migration test etc. of adjuvant, bonding agent, ink in addition.
Silicon rubber is as a large class of elastomeric material, because it has stable silica chemical constitution, the performance of elastic body uniqueness can be given, comprise biocompatibility, heat-resisting quantity, chemical-resistance, ageing-resistant performance, physiological inertia etc., and it is shorter with silicon rubber to be that starting material carry out rubber production cycle of processing and manufacturing, have higher throughput rate, therefore silastic product has been widely used in food contact material.Phenyl three (trimethylsiloxane group) silane (cas number is 9076-37-3 or 2116-84-9) is mainly used in skin care item, suncream, cosmetics, hair-care agent and anti-sweat deodorant etc., also be extensively present in silicon rubber, the method for testing therefore setting up phenyl three (trimethylsiloxane group) silane in a set of mensuration Food Contact silastic material is very necessary.
[summary of the invention]
For solving the problem, the invention provides a kind of method measuring phenyl three (trimethylsiloxane group) silane in Food Contact silastic material, this assay method sampling amount is few, pre-treatment is simple to operate, test fast, and can realize the Accurate Determining of phenyl three (trimethylsiloxane group) silane in Food Contact silastic material.
A kind of method measuring phenyl three (trimethylsiloxane group) silane in Food Contact silastic material, comprises the following steps:
1) sample pretreatment: testing sample is cut into the cube being not more than 2 × 2 × 2mm;
2) sample extraction: take appropriate amount of sample in ml headspace bottle, add acetone, covers tightly after bottle cap and places 10 hours under normal temperature, then by its ultrasonic extraction 4 hours under 25 degrees Celsius, finally gained extract is crossed 0.45 μm of PTFE filter membrane;
3) sample test: adopt gas chromatograph-mass spectrometer determination step 2) gained solution in the content of phenyl three (trimethylsiloxane group) silane, adopt quantified by external standard method, the condition determination of gas chromatograph-mass spectrometer is:
(1) gas chromatographic column adopts DB-5MS capillary column, and specification is column length 30 meters, column internal diameter 0.25 millimeter, thickness 0.25 micron;
(2) gas chromatographic sample introduction mouth temperature is set as 260 DEG C, and temperature programme is initial temperature 40 DEG C, retains 3 minutes, is warmed up to 100 DEG C by 10 DEG C per minute, be warmed up to 300 DEG C afterwards by 15 DEG C per minute, retains 1 minute;
(3) mass spectrum collection adopts and selects full scan and Selective ion mode scan mode to carry out simultaneously, and scan ion is m/z135, m/z207, m/z269.
Step 3) in, the retention time of sample peak with standard items peak is compared, and sample peak mass spectrogram is compared with standard substance mass spectrogram, if identical with standard substance, then contain phenyl three (trimethylsiloxane group) silane in confirmatory sample, adopt typical curve quantified by external standard method, computing formula is as follows:
wherein,
The machine-readable number (μ g/mL) of C---phenyl three (trimethylsiloxane group) silane,
V---final constant volume (mL),
W---example weight (g),
DF---extension rate.
Beneficial effect of the present invention: the present invention is that one utilizes the ultrasonic extraction of organic solvent, gas chromatograph-mass spectrometer is adopted to measure the method for phenyl three (trimethylsiloxane group) silane contents in Food Contact silastic material, this assay method sampling amount is few, pre-treatment is simple to operate, test fast, and the Accurate Determining of phenyl three (trimethylsiloxane group) silane in Food Contact silastic material can be realized, detecting of the method is limited to 40mg/kg, avoid Food Contact silastic material in the process contacted with food, objectionable constituent phenyl three (trimethylsiloxane group) silane in material may discharge or move in food, thus threat is brought to the physical and mental health of people.
[accompanying drawing explanation]
Fig. 1 is the gas chromatogram of phenyl three (trimethylsiloxane group) silane in embodiment;
Fig. 2 is the mass spectrogram of phenyl three (trimethylsiloxane group) silane in embodiment.
[specific embodiment]
One of the present invention measures the method for phenyl three (trimethylsiloxane group) silane in Food Contact silastic material, comprises the following steps:
1) sample pretreatment: testing sample is cut into the cube being not more than 2 × 2 × 2mm, this testing sample is Food Contact silastic material, and test substance is phenyl three (trimethylsiloxane group) silane;
2) sample extraction: take appropriate amount of sample in ml headspace bottle, adds Extraction solvent acetone, covers tightly after bottle cap and places 10 hours under normal temperature, then by its ultrasonic extraction 4 hours under 25 degrees Celsius, finally gained extract is crossed 0.45 μm of PTFE filter membrane;
3) sample test: adopt gas chromatograph-mass spectrometer determination step 2) gained solution in the content of phenyl three (trimethylsiloxane group) silane, adopt quantified by external standard method; Be specially, the retention time of sample peak with standard items peak is compared, and sample peak mass spectrogram is compared with standard substance mass spectrogram, if identical with standard substance, then contain phenyl three (trimethylsiloxane group) silane in confirmatory sample, adopt typical curve quantified by external standard method, computing formula is as follows:
wherein,
The machine-readable number (μ g/mL) of C---phenyl three (trimethylsiloxane group) silane,
V---final constant volume (mL),
W---example weight (g),
DF---extension rate.
Step 3) in, the condition determination of gas chromatograph-mass spectrometer is:
1) gas chromatographic column adopts DB-5MS capillary column, and specification is column length 30 meters, column internal diameter 0.25 millimeter, thickness 0.25 micron;
2) gas chromatographic sample introduction mouth temperature is set as 260 DEG C, and temperature programme is initial temperature 40 DEG C, retains 3 minutes, is warmed up to 100 DEG C by 10 DEG C per minute, be warmed up to 300 DEG C afterwards by 15 DEG C per minute, retains 1 minute;
3) mass spectrum collection adopts and selects full scan and Selective ion mode scan mode to carry out simultaneously, and scan ion is m/z135, m/z207, m/z269.
Below in conjunction with specific embodiment, following further illustrating is done to the present invention:
The mensuration of phenyl three (trimethylsiloxane group) silane in silastic material
1. the preparation of sample:
Testing sample is cut into the small cubes being not more than 2 millimeters × 2 millimeters × 2 millimeters, take the sample of 100mg in the ml headspace bottle of a 50mL, add 4mL acetone, place 10 hours under normal temperature after covering tightly bottle cap, then by its ultrasonic extraction 4 hours under 25 degrees Celsius, finally gained extract is crossed 0.45 μm of PTFE filter membrane.
2. set instrument parameter:
1) gas chromatograph condition
Gas chromatograph: Agilent6890
Chromatographic column: DB-5MS capillary column (30m × 0.25mm × 0.25 μm)
Injector temperature: 260 DEG C
Flow rate of carrier gas: 1.0mL/min, constant current
Sample introduction pattern: Splitless injecting samples
Sampling volume: 1 μ L
Temperature programme: initial temperature 40 DEG C, retains 3 minutes, is warmed up to 100 DEG C by 10 DEG C per minute, be warmed up to 300 DEG C afterwards by 15 DEG C per minute, retains 1 minute
2) Mass Spectrometry Conditions
Solvent delay: 4min
Acquisition mode: SCAN pattern and SIM pattern are carried out simultaneously
Ion source temperature: 230 DEG C
Quadrupole rod temperature: 150 DEG C
SCAN scan ion (m/z): 50 ~ 500
SIM scan ion (m/z): 135,207,269
3. quantitative and qualitative analysis
1) qualitative
Retention time through sample peak with standard items peak is compared, and sample peak mass spectrogram is compared with standard substance mass spectrogram, determines whether detect determinand in sample.
2) quantitative
Adopt typical curve quantified by external standard method
4. calculate
Computing formula is as follows:
The machine-readable number (μ g/mL) of C---phenyl three (trimethylsiloxane group) silane
V---final constant volume (mL)
W---example weight (g)
DF---extension rate.
The present invention, by the restriction of above-mentioned embodiment, change, the modification done, substitutes, combines, simplifies under other any does not deviate from Spirit Essence of the present invention and principle, all should be equivalent substitute mode, is included within protection scope of the present invention.
Claims (2)
1. measure a method for phenyl three (trimethylsiloxane group) silane in Food Contact silastic material, it is characterized in that, comprise the following steps:
1) sample pretreatment: testing sample is cut into the cube being not more than 2 × 2 × 2mm;
2) sample extraction: take appropriate amount of sample in ml headspace bottle, add acetone, covers tightly after bottle cap and places 10 hours under normal temperature, then by its ultrasonic extraction 4 hours under 25 degrees Celsius, finally gained extract is crossed 0.45 μm of PTFE filter membrane;
3) sample test: adopt gas chromatograph-mass spectrometer determination step 2) gained solution in the content of phenyl three (trimethylsiloxane group) silane, adopt quantified by external standard method, the condition determination of gas chromatograph-mass spectrometer is:
(1) gas chromatographic column adopts DB-5MS capillary column, and specification is column length 30 meters, column internal diameter 0.25 millimeter, thickness 0.25 micron;
(2) gas chromatographic sample introduction mouth temperature is set as 260 DEG C, and temperature programme is initial temperature 40 DEG C, retains 3 minutes, is warmed up to 100 DEG C by 10 DEG C per minute, be warmed up to 300 DEG C afterwards by 15 DEG C per minute, retains 1 minute;
(3) mass spectrum collection adopts and selects full scan and Selective ion mode scan mode to carry out simultaneously, and scan ion is m/z135, m/z207, m/z269.
2. a kind of method measuring phenyl three (trimethylsiloxane group) silane in Food Contact silastic material as claimed in claim 1, it is characterized in that, step 3) in, the retention time of sample peak with standard items peak is compared, and sample peak mass spectrogram is compared with standard substance mass spectrogram, if identical with standard substance, then contain phenyl three (trimethylsiloxane group) silane in confirmatory sample, adopt typical curve quantified by external standard method, computing formula is as follows:
The content of phenyl three (trimethylsiloxane group) silane
wherein,
Machine-readable several μ g/mL of C---phenyl three (trimethylsiloxane group) silane,
V---final constant volume mL,
W---example weight g,
DF---extension rate.
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