CN106501410A - The detection method of N nitrosodiethanolamines in a kind of cosmetics - Google Patents
The detection method of N nitrosodiethanolamines in a kind of cosmetics Download PDFInfo
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- CN106501410A CN106501410A CN201610957640.0A CN201610957640A CN106501410A CN 106501410 A CN106501410 A CN 106501410A CN 201610957640 A CN201610957640 A CN 201610957640A CN 106501410 A CN106501410 A CN 106501410A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N30/08—Preparation using an enricher
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
- G01N2030/062—Preparation extracting sample from raw material
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Abstract
The present invention relates in a kind of cosmetics N nitrosodiethanolamines detection method, and in particular to a kind of gas-chromatography thermal energy analyzer method for combined use of the N nitrosodiethanolamines in cosmetics, step is：N nitrosodiethanolamines are extracted from sample under ultrasound condition by cosmetics using water and chloroform mixed solution, after high speed refrigerated centrifuge, silicagel column is purified, and is detected with the solution obtained after methyl alcohol dissolution filter gas-chromatography thermal energy analyzer combination method after acetone eluant；The present invention can the N nitrosodiethanolamines that go out in water-soluble or fat-soluble cosmetics of effective detection, impurity peaks are few, and matrix interference is little, accurately, sensitivity is high, disclosure satisfy that the detection of N nitrosodiethanolamines in the dissimilar cosmetics such as creams class, aqua class, shampoo class.
Description
Technical field
The present invention relates in a kind of cosmetics and raw material N- nitrosodiethanolamines detection method.
Background technology
N- nitrosamine compounds are the strong chemical carcinogens of a class, can induce the malignant tumour of many animals.Make up
Product can reside in the positions such as skin, hair, nail, lip for a long time as articles for daily use, and its security receives much concern, and make up
N- nitrosamine in product is subject to strict both at home and abroad monitoring.At present, N- nitrosamine compounds of greatest concern in cosmetics are that N- is sub-
Nitro diethanol amine, used as the classification according to international cancer research institution (IARC), N- nitrosodiethanolamines range possibility
To human carcinogen.Due to widely used diethanol amine in cosmetics and triethanolamine this two classes material as cosmetics in moisturizing
Agent, pH poising agents or mixed with laurate as cosmetics in emulsifying agent and dispersant use, and diethanol amine and three ethanol
Both usual materials of amine are easy in Cosmetic Manufacture, storage and intermediate links to generate N- nitrosodiethanolamines, therefore
The detection of the N- nitrosodiethanolamines in cosmetics and control are subject to extensive concern both domestic and external, China to exist《Cosmetics health
Specification》In N- nitrosamine has clearly been classified as disabling component in cosmetics.
N- nitrosodiethanolamines are a kind of oily liquids of clear yellow viscous, belong to fixedness nitrosamine.Due to making up
In product, contained substance species is various, and especially the content of many nitrogen substances is far above N- nitrosodiethanolamines, is therefore making up
The detection tool of the N- nitrosodiethanolamines in product acquires a certain degree of difficulty.Carry out some N- for different cosmetics at present both at home and abroad
The detection method of nitrosodiethanolamine, such as gas chromatography mass spectrometry, gas-chromatography, liquid chromatography and Liquid Chromatography/Mass Spectrometry etc..Often at present
Using ISO/DIS15819-2013 methods be LC-MS method, but the method is easily subject to other compositions in cosmetics
Interference, detects limit for height.
Content of the invention
For above-mentioned present situation, it is an object of the invention to provide a kind of for cosmetics in the detection of N- nitrosodiethanolamines
Pretreatment technology and analysis method, impurity peaks are few, and matrix interference is little, accurately, sensitivity high, disclosure satisfy that creams class, aqua
The detection of N- nitrosodiethanolamines in the dissimilar cosmetics such as class, shampoo class.
In order to achieve the above object, the technical solution adopted in the present invention is：
(1) 3～5g cosmetics are taken into 50mL etalon plug volumetric flasks, the sulfamic acid amine and chlorine of 0.9～1.5g is added
Change sodium mixture, add 5.4～9mL water and chloroform mixed solution and through ultrasonic extraction, obtain ultrasonic extraction liquid；
(2) above-mentioned ultrasonic extraction liquid is taken, after refrigerated centrifuge, 3～5mL supernatants is taken and is positioned over nitrogen on Nitrogen evaporator and dry up,
Residue chloroform and the acetone mixed solution dissolving of 3～5mL, cross solid-phase extraction column, with the chloroform and third of 6～10mL
Ketone mixed solution drip washing, 6～10mL acetone are eluted, and collect eluent in test tube, and nitrogen is dried up, after the dissolving of 0.6～1mL methyl alcohol
With 0.20 μm of filtering with microporous membrane, the solution after being purified is stand-by in brown chromatogram bottle；
(3) N- in the solution after gas-chromatography-thermal energy analyzer method for combined use determination step (2) gained purification is sub-
Nitro diethanol amine, GC conditions are：Gas chromatographic column adopts middle polarity chromatographic column, and carrier gas is helium；Gas-chromatography
Column temperature adopts temperature programming.
The mixture sulfamic acid amine added in step (1) and the mass ratio of sodium chloride are 1:2.
In step (1), the volume ratio of water and chloroform mixed solution is 5:4.
In step (1), water is ultra-pure water of the resistivity more than 18M Ω * cm.
The refrigerated centrifuge condition of step (2) is：4 DEG C of cryogenic temperature, rotating speed 12000r/min, centrifugation time 15～
20min.
It is 5 to be used for dissolved residue and the chloroform of drip washing and the volume ratio of acetone mixed solution in step (2):1.
Solid-phase extraction column in step (2) is 2～3 silica gel of filling and the activated rear anhydrous sulphur of 3～5g of top loading
The glass packed column of sour sodium.
In step (3), testing conditions are, gas chromatograph：250 DEG C of injector temperature, 2 μ L of sample size, dottle pin are purged
15mL/min, chromatographic column adopt middle polarity chromatographic column, and flow rate of carrier gas 2.1mL/min, gas-chromatography column temperature adopt temperature programming：
150 DEG C of holding 10min of initial temperature, 10 DEG C/min rise to 230 DEG C of holding 2min, 250 DEG C of holding 3min；Thermal energy analyzer is detected
The condition of instrument is：250 DEG C of interface temperature, 600 DEG C of cracker temperature, ozone flow 10mL/min, -20 DEG C of chilling temperature, voltage
760V.
Beneficial effect of the present invention：The present invention relates to contained N- nitroso diethanols in the cosmetics of people's directly contact
Amine, establishes gas-chromatography thermal energy analyzer combination detection method.The present invention is to contained N- nitroso diethyls in cosmetics
The detection of hydramine is limited to 20 μ g/kg, and the method rate of recovery is 87～105%, and relative standard deviation is less than 10%.The invention impurity is done
Disturb little, the rate of recovery is high, and method is stable, can provide for the detection of N- nitrosodiethanolamines and control of product quality in cosmetics
Technical method support, disclosure satisfy that N- nitrosodiethanolamines in the dissimilar cosmetics such as creams class, aqua class, shampoo class
Detection.
Description of the drawings
Fig. 1 is inventive samples process chart；
Fig. 2 is N- nitrosodiethanolamines in cosmetics, before (a) being silica gel column chromatography, (b) for after silica gel column chromatography.
Specific embodiment
Below in conjunction with the accompanying drawings and specific embodiment is discussed in detail the present invention.But below example is only limitted to explain this
Bright, protection scope of the present invention should include the full content of claim, be not limited only to the present embodiment.
The step of embodiment of the present invention is：Utilize water and chloroform mixed solution under ultrasound condition by N- in cosmetics
Nitrosodiethanolamine is extracted from sample, and after high speed refrigerated centrifuge, silicagel column is purified, after acetone eluant
Detected with the solution obtained after methyl alcohol dissolution filter gas-chromatography-thermal energy analyzer combination method, can effective detection go out
N- nitrosodiethanolamines in water-soluble or fat-soluble cosmetics.Specific as follows：
1st, reagent and material
Except in addition explanation, it is pure that agents useful for same is analysis.
1.1N- nitrosodiethanolamines (N-Nitrosodiethanolamine)：Purity is more than 97%；
1.2 water：Ultra-pure water；
1.3 dichloromethane：Chromatographic grade；
1.4 methyl alcohol；
1.5 sulfamic acid amine；
1.6 chloroform；
1.7 helium：Concentration 99.999%
1.8 oxygen：Concentration 99.999%
1.9 acetone；
1.10 anhydrous sodium sulfate；
1.11 silica gel；
1.12N- nitrosodiethanolamine titer：Weigh N- nitrosodiethanolamine 1mg (being accurate to 0.0001g) standards
Product, are placed in 10mL brown volumetric flasks, add methyl alcohol to scale, and ultrasonic 10min helps dissolve, and the solution concentration is：100μg/
ML, keeps in dark place at -20 DEG C, 3 months shelf-lifves；
2nd, instrument and equipment
2.1 gas-chromatography：It is furnished with shunting/Splitless injecting samples mouth；
2.2 balance：Sensibility reciprocal 0.0001g；
2.3 refrigerated centrifuge：Rotating speed is not less than 12000r/min, and cryogenic temperature is not less than 0 DEG C；
2.4 ultrasound bath instrument
2.5 Nitrogen evaporator
2.6 pairs of property filter membranes
2.7 thermal energy analyzer detectors：Configuration heat cracker, cracking temperature are not less than 600 DEG C；
3rd, implementation steps, as shown in Figure 1.
3.1 extract
5g (being accurate to 0.0001g) sample is taken in 50mL conical flask with cover, adds sulfamic acid amine 0.5g (to be accurate to
0.0001g) with sodium chloride 1g (being accurate to 0.0001g), 5mL ultra-pure waters and 4mL chloroforms, ultrasonic extraction 30 under room temperature are added
15mL centrifuge tubes are transferred to after minute, 12000r/min refrigerated centrifuges 15min at 4 DEG C pipettes 5mL supernatants with 5mL pipettes
Liquid in test tube is positioned over nitrogen on Nitrogen evaporator and dries up, residue 5mL chloroforms and acetone (volume ratio 5:1) mixed solution
To be clean after dissolving.
3.2 purify
Make silica gel column chromatography：Silica gel and anhydrous sodium sulfate are dried to activate 10 hours at 110 DEG C and are protected in drier
Deposit.When making silica gel column chromatography, the silica gel dry pack after 3g activation is weighed in glass chromatography column, glass bar strikes reality, top layer
Anhydrous sodium sulfate after 5g activation is added, reality is struck.
3.1 liquid to be clean are transferred to silica gel column chromatography.With 10mL chloroforms and acetone (volume ratio 5：1) solution
Drip washing, 10mL acetone are eluted, and collect eluent in test tube, and nitrogen is dried up, and pipettor pipettes 1mL methyl alcohol dissolved residues, 0.20 μ
M filtering with microporous membrane in 2mL brown chromatogram bottles keeps in dark place at -20 DEG C and treats sample introduction.
Silica gel column chromatography column purification can effectively eliminate impurity interference in cosmetics, see Fig. 2, before (a) being silica gel column chromatography,
B () is silica gel column chromatography after, it can be seen that there was only N- nitrosodiethanolamines in the chromatogram after silica gel column chromatography column purification
Signal.
3.3 determine
3.3.1 GC conditions
Consideration different model gas chromatograph, following general technical specifications when providing gas chromatographic analysis.
1) chromatographic column：DB-624 quartz capillary columns, 30m × 0.32mm (i.d.) × 1 μm；
2) column temperature adopts temperature programming：150 DEG C of holding 10min of initial temperature, 10 DEG C/min rise to 230 DEG C of holding 2min,
250 DEG C of holding 3min；
3) carrier gas：Helium
4) flow rate of carrier gas：2.1mL/min；
5) injector temperature：250℃；
6) sample size：2μL；
7) dottle pin purging 15mL/min.
3.3.2 thermal energy analyzer analysis condition
1) interface temperature：250℃；
2) cracker temperature：600℃；
3) oxygen gas flow rate：10mL/min；
4) chilling temperature：-15℃；
5) detector voltage：760V.
3.3.3N- nitrosodiethanolamine calibration curve
Adopt accurate standard solution (100 μ g/mL) be configured to concentration for 50ng/mL, 100ng/mL, 200ng/mL,
The N- nitrosodiethanolamine solution of 500ng/mL, 1000ng/mL, 10000ng/mL, takes 2 μ L respectively in above-mentioned instrument experiment bar
It is measured under part, calibration curve is drawn to concentration with peak area.
3.3.4N- nitrosodiethanolamine cubage method
The present invention adopts external standard method, computing formula such as formula (1)
W in formula：Mass fraction (the unit of the N- nitrosodiethanolamines in cosmetics：Milligrams per kilogram；mg/kg)；
c：Concentration (the unit of N- nitrosodiethanolamines in the sample obtained by calibration curve：Milligrams per liter；mg/L))
V：Sample constant volume (unit：Rise；L)
m：Sample quality (unit：Gram；g)
4th, the linear equation and detection limit of method
Adopt accurate standard solution (100 μ g/mL) be configured to concentration for 50ng/mL, 100ng/mL, 200ng/mL,
The N- nitrosodiethanolamine solution of 500ng/mL, 1000ng/mL, 10000ng/mL, takes 2 μ L respectively in above-mentioned instrument experiment bar
It is measured under part, calibration curve is drawn to concentration (X-axis) with peak area (Y-axis), linear equation is obtained.
Table one：N- nitrosodiethanolamine calibration curves
5th, the rate of recovery and precision of method
The rate of recovery is tested, and is set three and is added concentration according to above-mentioned sample-pretreating method and experiment condition measure,
Each concentration carries out 6 tests, and the rate of recovery and precision of computational methods.As a result the rate of recovery 87～105%., calculate accurate
Degree (relative standard deviation RSD) the results are shown in Table two less than 10%.
Table two：The different recovery of standard addition of N- nitrosodiethanolamines and precision
6th, conclusion
For the present invention relates to N- nitrosodiethanolamines contained in cosmetics with people's directly contact, establish gas phase
Chromatogram thermal energy analyzer is combined detection method.By to different sample recovery rates, precision is tested, during the method is to cosmetics
The detection of contained N- nitrosodiethanolamines is limited to 20 μ g/kg, and the method rate of recovery is 87～105%, and relative standard deviation is little
In 10%.The invention impurity interference is little, and the rate of recovery is high, and method is stable, can be the inspection of N- nitrosodiethanolamines in cosmetics
Survey and control of product quality provides technical method and supports.
It should be noted that according to the above embodiment of the present invention, those skilled in the art are to realize the present invention completely
The four corner of independent claims and appurtenance, realize process and the same above-described embodiment of method.And the present invention is not detailed
Elaboration partly belongs to techniques well known.
General principle, principal character and the advantages of the present invention of the present invention has been shown and described above.The technology of this area
It should be appreciated that the present invention is not limited by examples detailed above, the various changes and modifications made by the present invention should both fall within will for personnel
Ask in the scope of the invention of protection.The claimed scope of the invention is defined by appending claims and its equivalent.
Claims (8)
1. in a kind of cosmetics N- nitrosodiethanolamines detection method, it is characterised in that comprise the following steps：
(1) 3～5g cosmetics are taken into 50mL etalon plug volumetric flasks, the sulfamic acid amine and sodium chloride of 0.9～1.5g is added
Mixture, adds 5.4～9mL water and chloroform mixed solution and through ultrasonic extraction, obtains ultrasonic extraction liquid；
(2) above-mentioned ultrasonic extraction liquid is taken, after refrigerated centrifuge, 3～5mL supernatants is taken and is positioned over nitrogen on Nitrogen evaporator and dry up, residue
Dissolved with the chloroform and acetone mixed solution of 3～5mL, cross solid-phase extraction column, mixed with the chloroform and acetone of 6～10mL
Solution drip washing is closed, 6～10mL acetone is eluted, eluent is collected in test tube, nitrogen is dried up, use after the dissolving of 0.6～1mL methyl alcohol
0.20 μm of filtering with microporous membrane, is purified rear solution stand-by in brown chromatogram bottle；
(3) the N- nitrosos two in solution after gas-chromatography-thermal energy analyzer method for combined use determination step (2) gained purification
Monoethanolamine, GC conditions are：Gas chromatographic column adopts middle polarity chromatographic column, and carrier gas is helium；Gas-chromatography column temperature is adopted
Use temperature programming.
2. detection method according to claim 1, it is characterised in that：The mixture amino sulphur added in step (1)
The mass ratio of acid amide and sodium chloride is 1:2.
3. detection method according to claim 1, it is characterised in that：In step (1), water and chloroform mixing are molten
The volume ratio of liquid is 5:4.
4. the detection method according to claim 1 or 3, it is characterised in that：In step (1), water is more than for resistivity
The ultra-pure water of 18M Ω * cm.
5. detection method according to claim 1, it is characterised in that：The refrigerated centrifuge condition of step (2) is：Freezing
4 DEG C of temperature, rotating speed 12000r/min, 15～20min of centrifugation time.
6. detection method according to claim 1, it is characterised in that：It is used for dissolved residue and drip washing in step (2)
Chloroform and acetone mixed solution volume ratio be 5:1.
7. detection method according to claim 1, it is characterised in that：Solid-phase extraction column in step (2) is filling 2
～3 silica gel and the glass packed column of the activated rear anhydrous sodium sulfates of 3～5g of top loading.
8. detection method according to claim 1, it is characterised in that：In step (3), testing conditions are, gas-chromatography
Instrument：250 DEG C of injector temperature, 2 μ L of sample size, dottle pin purge 15mL/min, and chromatographic column adopts middle polarity chromatographic column, carrier gas stream
Fast 2.1mL/min；Gas-chromatography column temperature adopt temperature programming for：150 DEG C of holding 10min of initial temperature, 10 DEG C/min rise to 230
DEG C keep 2min, 250 DEG C holding 3min；Thermal energy analyzer condition is：250 DEG C of interface temperature, 600 DEG C of cracker temperature, ozone
Flow 10mL/min, -20 DEG C of chilling temperature, voltage 760V.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760917A (en) * | 2018-05-24 | 2018-11-06 | 中国烟草总公司郑州烟草研究院 | One grow tobacco and the processing method of tobacco product, tobacco and tobacco product in N- nitrosodiethanolamine contents assay method |
| CN110161148A (en) * | 2019-06-20 | 2019-08-23 | 武夷学院 | The pre-treating method and content analysis method of perchlorate in a kind of food |
| CN112730663A (en) * | 2020-12-22 | 2021-04-30 | 华测检测认证集团湖北有限责任公司 | Method for rapidly and accurately measuring volatile nitrosamine in food |
| CN114942295A (en) * | 2022-04-28 | 2022-08-26 | 上海市食品药品检验研究院 | Method for extracting and detecting total nitrosamines in cosmetics |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108760917A (en) * | 2018-05-24 | 2018-11-06 | 中国烟草总公司郑州烟草研究院 | One grow tobacco and the processing method of tobacco product, tobacco and tobacco product in N- nitrosodiethanolamine contents assay method |
| CN108760917B (en) * | 2018-05-24 | 2020-11-24 | 中国烟草总公司郑州烟草研究院 | Tobacco and tobacco product treatment method and method for measuring content of N-nitrosodiethanolamine in tobacco and tobacco product |
| CN110161148A (en) * | 2019-06-20 | 2019-08-23 | 武夷学院 | The pre-treating method and content analysis method of perchlorate in a kind of food |
| CN112730663A (en) * | 2020-12-22 | 2021-04-30 | 华测检测认证集团湖北有限责任公司 | Method for rapidly and accurately measuring volatile nitrosamine in food |
| CN114942295A (en) * | 2022-04-28 | 2022-08-26 | 上海市食品药品检验研究院 | Method for extracting and detecting total nitrosamines in cosmetics |
| CN114942295B (en) * | 2022-04-28 | 2023-12-22 | 上海市食品药品检验研究院 | Method for extracting and detecting total nitrosamine in cosmetics |
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Address after: Two West Road Lake Development Zone in Tongling City, Anhui province 244061 No. 1517 building 4 room 208 Applicant after: ANHUI YIKANGDA PHOTOELECTRIC TECHNOLOGY CO., LTD. Applicant after: Hefei Research Institute of product quality supervision and inspection Applicant after: Hefei Inst. of Matter Sciences, Chinese Academy of Sciences Address before: Two West Road Lake Development Zone in Tongling City, Anhui province 244061 No. 1517 building 4 room 208 Applicant before: ANHUI YIKANGDA PHOTOELECTRIC TECHNOLOGY CO., LTD. Applicant before: Hefei Institute of product quality supervision and inspection Applicant before: Hefei Inst. of Matter Sciences, Chinese Academy of Sciences |
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Application publication date: 20170315 |
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| WD01 | Invention patent application deemed withdrawn after publication |