CN105259281B - The assay method of karanal content in a kind of plastic toy material - Google Patents
The assay method of karanal content in a kind of plastic toy material Download PDFInfo
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- CN105259281B CN105259281B CN201510436006.8A CN201510436006A CN105259281B CN 105259281 B CN105259281 B CN 105259281B CN 201510436006 A CN201510436006 A CN 201510436006A CN 105259281 B CN105259281 B CN 105259281B
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Abstract
The invention discloses a kind of assay methods of karanal content in plastic toy material, belong to analysis technical field, and the method for measuring karanal content in plastic toy material is combined more particularly, to a kind of gas chromatography mass spectrometer, is included the following steps：By sample comminution, mixing, uniform sample to be tested, N, the dissolving of N dimethylformamides, 80 DEG C of balance 30min, static headspace-GC-MS instrument combination measurement, quantified by external standard method are weighed.Content of the method using the present invention suitable for measuring karanal plastic toy material, it is simple and convenient, there is higher precision.
Description
Technical field
The invention belongs to analysis technical field, it is related to a kind of assay method of karanal content in plastic toy material,
The method for measuring karanal content in plastic toy material is combined more particularly, to a kind of gas chromatograph-mass spectrometer.
Background technology
Karanal also known as 2- (2,4- dimethyl -3- cyclohexyl) -5- methyl -5- (1- methyl-propyls) -1,3- dioxies are disliked
Alkane, 2- (4,6- dimethyl -3- cyclohexyl) -5- methyl -5- (1- methyl-propyls) -1,3- dioxy oxanes, two kinds of structures are card
The relatively conventional isomer of garland aldehyde, See Figure.
Karanal can be seen below there are many chiral isomer：
1,3-Dioxane, 2- (2,4-dimethyl-3-cyclohexen-1-yl) -5-methyl-5- (1-
methylpropyl)-
1,3-Dioxane, 2- [(1R, 2R) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, cis-rel-
1,3-Dioxane, 2- [(1R, 2R) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, trans-rel-
1,3-Dioxane, 2- [(1S, 2S) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, cis-
1,3-Dioxane, 2- [(1S, 2R) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, cis-
1,3-Dioxane, 2- [(1R, 2S) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, cis-
1,3-Dioxane, 2- [(1R, 2R) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, cis-
1,3-Dioxane, 2- [(1S, 2S) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, trans-
1,3-Dioxane, 2- [(1S, 2R) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, trans-
1,3-Dioxane, 2- [(1R, 2S) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, trans-
1,3-Dioxane, 2- [(1R, 2R) -2,4-dimethyl-3-cyclohexen-1-yl] -5-methyl-5- (1-
Methylpropyl)-, trans-
Karanal is colourless liquid, has strong dry, with saturating hair property wooden amber aroma, and lasting ability is strong, point
Minor C17H30O2, molecular weight 266.43, boiling point is higher than 250 DEG C, and 0.61 ± 0.06mg/L is (at 19.7-20.2 DEG C for water solubility；pH
7.7-8.1), it is to be widely used in the daily chemical products such as perfume, soap, washing powder with the fragrance raw material of dry imperial saliva root of Aucklandia lappa Decne.
Meanwhile it also has outstanding fabric lasting ability, is widely used in shampoo and fabric softening agent.In European Union, karanal
Have been cited as the 13rd batch high attention rate substances (SVHC) of European chemical balance motion office ECHA.
Currently, toy manufacturer is to exploit market, expand sales volume, research and develop diversification toy product, wherein tool fragrance is expected
Toy comes into being.In in the processing and making process of tool the expected toy of fragrance, often add lasting ability by force, thick taste
Spices and essence, and karanal is because lasting ability is strong and receives toy manufacturer favor with strong ambergris.However, card
Garland aldehyde may cause certain harm to human body and environment, be put into because having high persistence and high bioaccumulation
In the high concern list of substances of REACH the 13rd crowd, the addition of karanal will be by the toy trade for Europe inlet and outlet
The limitation of high degree.However, Chinese toy industry is largely exported towards European Union area, in order to cope with REACH regulations, has fragrant modeling
The detection of the content of karanal necessitates index in glue toy, so as to the stringent control toy during manufacturing
The content of karanal in finished product.
Currently, the researcher of related field stresses the synthesis and application in karanal, pertinent literature research and country
Standard not yet finds that be directed to plastic toy material detects karanal content method using HS GC Mass Spectrometry,
Therefore the present invention establish it is a kind of easily and efficiently detect plastic toy material in karanal content method have Chinese medicine meaning
Justice.
Invention content
Technical problem to be solved by the present invention lies in provide a kind of measurement of karanal content in plastic toy material
Method.To achieve the above object, the present invention takes following design scheme：
The method that HS GC Mass Spectrometry detects karanal content in plastic toy material includes following step
Suddenly：
By sample comminution, mixing.0.1-0.5 grams of uniform sample to be tested is weighed, organic solvent N, N- dimethyl formyl is added
Amine 10ml is balanced 30 minutes, is measured with HS GC mass spectrometer, specific instrument condition in 80 DEG C of temperature
For：
Carrier gas：Helium；
Flow rate of carrier gas：1.00ml/min；
Chromatographic column：DB-5,15m × 0.25mm × 0.1 μm；
Sampling system：Head space
Sample size：1ml；
Injector temperature：270℃；
Transmission line temperature：280 DEG C,
Column temperature：70 DEG C of holdings 2min, 20 DEG C/min are warming up to 290 DEG C, keep 10min；
MS conditions：EI；
230 DEG C of ion source temperature；
SIM modes scan；
Characteristic ion is m/z=120.0,157.0,107.0,266.0,69.0, wherein m/z=120.0 is quota ion.
Karanal standard items are weighed, uses methanol to dissolve and after constant volume as standard reserving solution, then further uses methanol
It is diluted to the standard solution with a certain concentration gradient, according to standard substance quality and response fit standard working curve；
Result of calculation, the calculation formula of karanal content is in sample
X=c/m
In formula：
The content of karanal in X- samples, unit are milligrams per kilogram (mg/kg)；
C- sample introduction samples concentration × sampling volume, unit are microgram (μ g)；
M- sample masses, unit are gram (g).
Preferably, 0.2 gram of sample to be tested is weighed
Preferably, the gradient of a concentration of 0.5,1.0,2.0,5,10 μ g of the standard solution uses liquid.
Preferably, described to be to the condition that sample treatment solution is detected using gas chromatography-mass spectrometry：Carrier gas：Helium
Gas；Flow rate of carrier gas：1.00ml/min；Chromatographic column：DB-5,15m × 0.25mm × 0.1 μm；Sample size：1ml；Injector temperature：
270℃；Transmission line temperature：280 DEG C, column temperature：70 DEG C of holdings 2min, 20 DEG C/min are warming up to 290 DEG C, keep 10min；
MS conditions：EI；230 DEG C of ion source temperature；SIM modes scan；And it is qualitative according to mass spectra peak, external standard peak area is legal
Amount.Characteristic ion：M/z=120.0,157.0,107.0,266.0,69.0；
Preferably, the external standard peak area method is quantitative, withM/z=120.0For quota ion.
Karanal standard substance (isomer) total ion current figure is shown in that Fig. 1, four kinds of isomer retention times exist
7.3-8.0min。
Effective effect：It is an advantage of the invention that：Karanal in method detection plastic toy material using the present invention
Content, quickly and effectively, RSD% are not more than 5%, and detection is limited to 0.02mg/kg.It can be seen that the method for the present invention, is played for detection
The detection for having karanal in material provides a kind of reliable method convenient to carry out, has higher precision and relatively low
Detection limit, disclosure satisfy that detection needs.
Description of the drawings
Fig. 1 karanal standard substance total ion current figures
Fig. 2 karanal standard substance mass spectrograms
Specific implementation mode
Embodiment 1, the detection of karanal content in polyethylene plastic toy：
Precision weighs karanal standard items (purity 95.5%) 13.09mg, and methanol dissolving and constant volume are 25.0mL, concentration
500mg/L is as storing solution, with 50 times, concentration 10mg/L of methanol dilution, then is diluted to the standard of 0.5,1.0,2.0,5,10 μ g
Use liquid.
Solid sample is crushed, mixing, uniform sample to be tested 0.2002g, accurate weighing is taken to be placed in head space to 0.0001 gram
In bottle, 10mL n,N-Dimethylformamide is added, is analyzed with head space-GC-MS after 80 DEG C of balance 30min.
Detecting instrument is Shimadzu GC/MS-QP2010 Ultra, matches HS-20 headspace sampling systems；
Testing conditions are：
Carrier gas：Helium；
Flow rate of carrier gas：1.00ml/min；
Chromatographic column：DB-5,15m × 0.25mm × 0.1 μm；
Sampling system：HS-20 headspace sampling systems
Sample size：1ml；
Injector temperature：270℃；
Transmission line temperature：280 DEG C,
Column temperature：70 DEG C of holdings 2min, 20 DEG C/min are warming up to 290 DEG C, keep 10min；
MS conditions：EI；
230 DEG C of ion source temperature；
SIM modes scan；
And it is qualitative according to mass spectra peak, external standard peak area method is quantitative.Characteristic ion：M/z=120.0, 157.0,107.0,
266.0,69.0；
The calculation formula of karanal content is in sample
X=c/m--------------------- (1)
In formula：
The content of karanal in X- samples, unit are milligrams per kilogram (mg/kg)；
C- sample introduction samples concentration × sampling volume, unit are microgram (μ g)；
M- sample masses, unit are gram (g).
By calculating, result is：
The content of karanal is calculated by formula (1) in sample, as a result as follows：
Principle and implementation of the present invention are described for specific case used herein, and above example is said
The bright method and its core concept for being merely used to help understand the present invention；Meanwhile for those of ordinary skill in the art, foundation
The thought of the present invention, there will be changes in the specific implementation manner and application range, in conclusion the content of the present specification is not
It is interpreted as limitation of the present invention.
Claims (2)
1. the assay method of karanal content in a kind of plastic toy material, it is characterised in that the assay method includes as follows
Step：
A. sample preparation：By sample comminution, mixing, 0.1-0.5 grams of uniform sample to be tested is weighed, it is molten that 10mL organic solvents are added
Solution, 80 DEG C balance 30 minutes, and HS GC mass spectrometer is measured；
B. working curve：Karanal standard items are weighed, series standard working solution, HS GC mass spectrometer are prepared
It is measured, linear fit；
C. HS GC mass spectrometer detects, and testing conditions are：
Carrier gas：Helium；
Flow rate of carrier gas：1.00ml/min；
Chromatographic column：DB-5,15m × 0.25mm × 0.1 μm；
Sampling system：Head space
Sample size：1ml；
Injector temperature：270℃；
Transmission line temperature：280 DEG C,
Column temperature：70 DEG C of holdings 2min, 20 DEG C/min are warming up to 290 DEG C, keep 10min；
MS conditions：EI；
230 DEG C of ion source temperature；
SIM modes scan：And, external standard method peak area quantification qualitative according to mass spectra peak, characteristic ion m/z=120.0,157.0,
107.0,266.0,69.0, wherein m/z=120.0 are quota ion；
D. it calculates
The calculation formula of karanal content is in sample
X=c/m
In formula：
The content of karanal in X- samples, unit are milligrams per kilogram (mg/kg)；
C- sample introduction samples concentration × sampling volume, unit are microgram (μ g)；
M- sample masses, unit are gram (g).
2. the assay method of karanal content in a kind of plastic toy material according to claim 1, it is characterised in that
Organic solvent described in sample preparation steps therein is n,N-Dimethylformamide.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999057233A1 (en) * | 1998-05-07 | 1999-11-11 | Quest International B.V. | Perfume composition |
| CN102432588A (en) * | 2011-11-25 | 2012-05-02 | 河南科技大学 | Method for synthesizing karanal |
| CN103215130A (en) * | 2013-03-14 | 2013-07-24 | 天津市双马香精香料新技术有限公司 | Perfume essence with karanal added |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2012001551A (en) * | 2003-09-09 | 2012-01-05 | Kao Corp | Deodorizing composition for hircismus, and skin cosmetic and deodorant for fiber, both containing the composition |
-
2015
- 2015-07-22 CN CN201510436006.8A patent/CN105259281B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO1999057233A1 (en) * | 1998-05-07 | 1999-11-11 | Quest International B.V. | Perfume composition |
| CN102432588A (en) * | 2011-11-25 | 2012-05-02 | 河南科技大学 | Method for synthesizing karanal |
| CN103215130A (en) * | 2013-03-14 | 2013-07-24 | 天津市双马香精香料新技术有限公司 | Perfume essence with karanal added |
Non-Patent Citations (4)
| Title |
|---|
| Volatile Substances in Polymer Toys Made from Butadiene and Styrene;Yutaka Abe et al.;《American Journal of Analytical Chemistry》;20130531;第4卷;第229页"ABSTRACT"，第230页首段，第230-231页2.1-2.5节 * |
| 顶空气相色谱-质谱法测定玩具中的10种挥发性有机物;吕庆 等;《色谱》;20100831;第28卷(第8期);800-804页 * |
| 香料卡拉花醛的全合成及工艺研究;张志新;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20140615(第6期);全文 * |
| 香料吐纳麝香和卡拉花醛的合成研究;吴秀芹;《中国优秀硕士学位论文全文数据库 工程科技Ⅰ辑》;20110930(第9期);全文 * |
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