CN108593786A - A kind of assay method of saualane content - Google Patents
A kind of assay method of saualane content Download PDFInfo
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- CN108593786A CN108593786A CN201810242162.4A CN201810242162A CN108593786A CN 108593786 A CN108593786 A CN 108593786A CN 201810242162 A CN201810242162 A CN 201810242162A CN 108593786 A CN108593786 A CN 108593786A
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- saualane
- sample
- ethyl acetate
- reference substance
- content
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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
-
- 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
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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
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
Abstract
The present invention relates to a kind of assay methods of saualane content, include the following steps：(1) prepared by reference substance solution：Saualane reference substance is taken, addition ethyl acetate, which dissolves, is made reference substance solution, and the volume ratio of the saualane reference substance and ethyl acetate is 1:5~20；(2) prepared by sample solution：Saualane sample is taken, is dissolved in addition ethyl acetate and sample solution is made, the volume ratio of the saualane sample and ethyl acetate is 1:5~20；(3) it measures：Saualane content in the sample solution obtained to step (2) using gas chromatography combined with mass spectrometry technology is measured.The content of gas-chromatography tandem mass spectrometry detection saualane provided by the invention, detection method sample extraction is easy, and easy to operate, quickly, the content of accurate qualitative and quantitative analysis saualane can effectively control the quality of saualane.
Description
Technical field
The present invention relates to technical field of analysis and detection, more particularly to a kind of assay method of saualane content.
Background technology
Saualane is the hydrogenated obtained a kind of squalene extracting haveing excellent performance of squalene extracted from hydrogenated hydro carbons grease,
It is also known as eepwater shark liver oils.Scientific research finds that saualane is that rare chemical stability is high, the splendid animal oil of use feeling
Fat has preferable compatibility to skin, will not cause allergy and stimulation, and can accelerate formula in other active components into skin
Infiltration；With lower polarity and medium spreadability, and pure, colourless, free from extraneous odour；It may also suppress the growth of mould.At present
Saualane is mainly used in cosmetic industry, since its skin effect is good, can reinforce maintenance epidermis, be effectively formed natural guarantor
Cuticula helps the balance between skin and sebum.It can also inhibit the peroxidating of skin lipid, can effectively infiltrate through skin, and promote
The proliferation of skin base cell, to delay skin aging, improving and eliminating chloasma has apparent physiologic effect.Skin can also be made
Skin pore opens, and promotes blood microcirculation, promotes the metabolism of cell, and damaged cell is repaired in help.
However the report at present about saualane detection is less, is concentrated mainly on the synthesis and application of saualane, for changing
The use of saualane is increasing in cosmetic industry, and the control of saualane quality is extremely urgent, and therefore, those skilled in the art compel
It is essential and wants a method for being suitable for saualane detection, this method can fast and accurately qualitative and quantitative analysis saualane contain
Amount.
Invention content
The object of the present invention is to provide a kind of assay methods of saualane content, and this method is easy to operate, quickly, accurate fixed
The content of property quantitative analysis saualane, can effectively control the quality of saualane.
The object of the present invention is to provide a kind of assay methods of saualane content, include the following steps：
(1) prepared by reference substance solution：Saualane reference substance is taken, ethyl acetate dissolving is added, reference substance solution is made, it is described
Saualane reference substance and ethyl acetate volume ratio be 1:5~20；
(2) prepared by sample solution：Saualane sample is taken, dissolving in ethyl acetate is added, sample solution, the angle is made
The volume ratio of shark alkane sample and ethyl acetate is 1:5~20；
(3) it measures：Saualane in the sample solution obtained to step (2) using Gas chromatographyMass spectrometry is contained
Amount is measured, and GC conditions are：Chromatographic column：Stationary phase is the capillary of -95% dimethyl polysiloxane of 5% phenyl
Column, size are 30m × 0.25mm × 0.5 μm；Column temperature：150 DEG C of holding 4min, 280 are warming up to the rate of 5~15 DEG C/min
DEG C, keep 3min；Column flow rate：1.0mL/min；Injector temperature：250℃；Detector temperature：250℃；Carrier gas：Helium；Sample introduction
Mode：Split sampling, split ratio 5:1；Sample size：1 μ L, Mass Spectrometry Conditions are：EI ion source temperatures：230℃；Level four bars temperature
Degree：150℃；Solvent delay 3min；Scan mode：SIM, it is 421 to select parent ion, daughter ion is respectively 29,43,57,71,
85、99、113、127、141、155、169、183、197、211、225、239、253、267、281、295、309、323、337、
351,365,379,393,407, reference substance solution and the corresponding chromatogram of sample solution and peak area are recorded, with quantified by external standard method
Calculate the content of saualane.
The present invention establishes a kind of simple, effective, practical saualane detection method, utilizes gas chromatography combined with mass spectrometry
Method, the content of accurate qualitative and quantitative analysis saualane can effectively control the quality of saualane.
Preferably, the volume ratio of the saualane reference substance described in step (1) and ethyl acetate is 1:10, in step (2)
The volume ratio of the saualane sample and ethyl acetate is 1:10.
Preferably, the column temperature described in step (3) is：150 DEG C of holding 4min, 280 are warming up to the rate of 5 DEG C/min
DEG C, keep 3min.
The method of the present invention overcomes the deficiency of prior art sample treatment, and compared with prior art, the present invention has
Following excellent results：The content of gas-chromatography tandem mass spectrometry detection saualane provided by the invention, the detection method sample carry
Simplicity is taken, easy to operate, quickly, the content of accurate qualitative and quantitative analysis saualane can effectively control the quality of saualane；
Reproducible, the requirement that recovery of standard addition satisfaction analysis measures of the method for the present invention；Gas chromatography is used to survey in the prior art
The content for determining saualane must possess saualane standard items since gas-chromatography is qualitative, carried out by retention time it is qualitative, and this
Invention propose gas-chromatography tandem mass spectrum rule do not need, by mass spectral analysis can qualitative saualane, be more convenient to spiny dogfish
Alkane sample carries out qualitative, has higher sensitivity with time gas chromatography tandem mass spectrum, can respond the concentration of nanogram level, and gas
The response of phase chromatography generally accomplishes Gamma Magnitude.
Description of the drawings
Fig. 1 is the saualane sample chromatogram figure that 1 extracting solution of embodiment is ethyl acetate；
Fig. 2 is the saualane sample chromatogram figure that 1 extracting solution of comparative example is methanol；
Fig. 3 is the saualane sample chromatogram figure that 2 extracting solution of comparative example is ethyl alcohol；
Fig. 4 is the saualane sample chromatogram figure for the polyethylene glycol capillary column that comparative example 3 is modified using nitroterephthalic acid；
Fig. 5 is saualane sample chromatogram of the comparative example 4 using -10% polyethylene glycol capillary column of dimethyl polysiloxane
Figure；
Fig. 6 is saualane sample chromatogram figure of the comparative example 5 using 100% dimethyl polysiloxane capillary column；
Fig. 7 is the saualane sample chromatogram figure of embodiment 4；
Fig. 8 is the saualane sample chromatogram figure of embodiment 5.
Specific implementation method
The present invention is further described by following specific examples, but does not limit the present invention.
Laboratory apparatus, reagent and operating condition
1) instrument
Agilent 7890B gas chromatographs are furnished with 5977B mass detectors (Agilent company of the U.S.)；WBK-4B type electricity
Hot thermostat water bath (Huankai Microbes Tech Co., Ltd., Guangdong)；Ultrasonic washing instrument (the limited public affairs of Shanghai Luxi analytical instrument
Department)；Centrifuge TDZ5-WS (Hunan C1-esteraseremmer-N Xiang Yi Science and Technology Ltd.s)；Micro-whirlpool mixed instrument XW-80A (is analyzed Shanghai Luxi
Instrument Ltd.)；Sartorius electronic balances (BSA224S) (Guangzhou Shen Hua experimental instrument and equipments Co., Ltd).
2) reagent
Saualane reference substance (German Dr.Ehrenstorfer companies, article No.：C16973500, content 99.5%), acetic acid
Ethyl ester, methanol, ethyl alcohol are chromatographically pure, are purchased from CNW scientific ＆ technical corporation of Germany.
3) chromatographic condition
Chromatographic column：Stationary phase is the capillary column of -95% dimethyl polysiloxane of 5% phenyl, and size is 30m × 0.25mm
×0.5μm；Column temperature：150 DEG C of holding 4min, are warming up to 280 DEG C with the rate of 5~15 DEG C/min, keep 3min；Column flow rate：
1.0mL/min；Injector temperature：250℃；Detector temperature：250℃；Carrier gas：Helium；Input mode：Split sampling, shunting
Than being 5:1；Sample size：1 μ L, Mass Spectrometry Conditions are：EI ion source temperatures：230℃；Level four bars temperature：150℃；Solvent delay
3min；Scan mode：SIM, it is 421 to select parent ion, daughter ion is respectively 29,43,57,71,85,99,113,127,141,
155、169、183、197、211、225、239、253、267、281、295、309、323、337、351、365、379、393、407。
Embodiment 1
As shown in Figure 1, a kind of assay method of saualane content, includes the following steps：
(1) prepared by reference substance solution：Saualane reference substance is added ethyl acetate dissolving and reference substance solution, saualane is made
The volume ratio of reference substance and ethyl acetate is 1:10；
(2) prepared by sample solution：Saualane sample is taken, dissolving in ethyl acetate is added, sample solution, saualane sample is made
The volume ratio of product and ethyl acetate is 1:10；
(3) it measures：Saualane in the sample solution obtained to step (2) using Gas chromatographyMass spectrometry is contained
Amount is measured, and GC conditions are：Chromatographic column：Stationary phase is the capillary of -95% dimethyl polysiloxane of 5% phenyl
Column, size are 30m × 0.25mm × 0.5 μm；Column temperature：150 DEG C of holding 4min, are warming up to 280 DEG C with the rate of 5 DEG C/min, protect
Hold 3min；Column flow rate：1.0mL/min；Injector temperature：250℃；Detector temperature：250℃；Carrier gas：Helium；Input mode：
Split sampling, split ratio 5:1；Sample size：1 μ L, Mass Spectrometry Conditions are：EI ion source temperatures：230℃；Level four bars temperature：150
℃；Solvent delay 3min；Scan mode：SIM, it is 421 to select parent ion, daughter ion is respectively 29,43,57,71,85,99,
113、127、141、155、169、183、197、211、225、239、253、267、281、295、309、323、337、351、365、
379,393,407, reference substance solution and the corresponding chromatogram of sample solution and peak area are recorded, spiny dogfish is calculated with quantified by external standard method
The content of alkane.
It may occur to persons skilled in the art that the sample containing saualane within protection scope of the present invention.
Comparative example 1
As shown in Fig. 2, it is same as Example 1, the difference is that：It is molten that methanol is added in saualane reference substance in step (1)
Solution is made reference substance solution, and the volume ratio of saualane reference substance and methanol is 1:10, first is added in saualane sample in step (2)
Alcohol, which dissolves, is made sample solution, and the volume ratio of saualane sample and methanol is 1:10.
Comparative example 2
As shown in figure 3, it is same as Example 1, the difference is that：It is molten that ethyl alcohol is added in saualane reference substance in step (1)
Solution is made reference substance solution, and the volume ratio of saualane reference substance and ethyl alcohol is 1:10, second is added in saualane sample in step (2)
Alcohol, which dissolves, is made sample solution, and the volume ratio of saualane sample and ethyl alcohol is 1:10.
Shown in chromatogram figure Fig. 1 that embodiment 1 obtains, peak shape is preferable, no hangover；The chromatogram that comparative example 1 obtains such as Fig. 2
Shown, chromatographic peak miscellaneous peak is more；Chromatogram that comparative example 2 obtains is as shown in figure 3, chromatography not appearance.
Comparative example 3
As shown in figure 4, it is same as Example 1, the difference is that：Chromatographic column changes for nitroterephthalic acid in step (3)
The polyethylene glycol capillary column of property.
Comparative example 4
As shown in figure 5, it is same as Example 1, the difference is that：Chromatographic column is dimethyl polysiloxane-in step (3)
10% polyethylene glycol capillary column.
Comparative example 5
As shown in fig. 6, it is same as Example 1, the difference is that：Chromatographic column is the poly- silicon of 100% dimethyl in step (3)
Oxygen alkane capillary column.
Compared to Figure 1 compared with the peak shape that Fig. 1 is obtained is preferable, no hangover, and the chromatogram that comparative example 3 obtains is as shown in figure 4, angle
Shark alkane chromatographic peak retention time has deviation, and miscellaneous peak is more；Chromatogram that comparative example 4 obtains as shown in figure 5, chromatography not appearance,
And spectrogram is poor；Chromatogram that comparative example 5 obtains is as shown in fig. 6, chromatographic peak profile is wider, peak overlap, and miscellaneous peak is more.
Embodiment 2
It is same as Example 1, the difference is that：The volume ratio of saualane reference substance and ethyl acetate is in step (1)
1:5；The volume ratio of saualane sample and ethyl acetate is 1 in step (2):5.
Embodiment 3
It is same as Example 1, the difference is that：The volume ratio of saualane reference substance and ethyl acetate is in step (1)
1:20；The volume ratio of saualane sample and ethyl acetate is 1 in step (2):20.
Saualane sample in embodiment 1, embodiment 2 and embodiment 3 is detected respectively, obtained result such as 1 institute of table
Show.
Table 1
It can be obtained by table 1, the volume ratio of saualane sample and ethyl acetate is less than 1：10 or be more than 1：When 10, extraction
Rate reduces, and is unfavorable for the measurement of saualane content.
Embodiment 4
As shown in fig. 7, it is same as Example 1, the difference is that：Column temperature is in step (3)：60 DEG C of holding 1min, with
The rate of 15 DEG C/min is warming up to 200 DEG C, then is warming up to 280 DEG C with the rate of 13 DEG C/min, keeps 3min.
Embodiment 5
As shown in figure 8, it is same as Example 1, the difference is that：Column temperature is in step (3)：120 DEG C of holding 4min, with
The rate of 15 DEG C/min is warming up to 200 DEG C, then is warming up to 280 DEG C with the rate of 13 DEG C/min, keeps 3min.
By Fig. 1 compared with Fig. 7 and Fig. 8, saualane chromatographic peak retention time is deviated in Fig. 7, and saualane does not go out in Fig. 8
Peak, and spectrogram is poor.
Embodiment 6
Repeatability and sample recovery rate experiment：
Mark-on reclaims are carried out to raw material saualane used for cosmetic respectively with gas-chromatography tandem mass spectrometry and gas chromatography
Rate is tested, and comparing result is shown in Table 2.As shown in Table 2, gas-chromatography tandem mass spectrometry collimation, accuracy are above gas-chromatography
Method.
2 gas-chromatography tandem mass spectrometry of table and gas chromatography results contrast
Tab.2 Comparison of GC-MS and GC
Above-listed detailed description is illustrating for possible embodiments of the present invention, which is not to limit this hair
Bright the scope of the claims, all equivalence enforcements or change without departing from carried out by the present invention are intended to be limited solely by the scope of patent protection of this case
In.
Claims (4)
1. a kind of assay method of saualane content, which is characterized in that include the following steps：
(1) prepared by reference substance solution：Saualane reference substance is taken, ethyl acetate dissolving is added, reference substance solution, the angle is made
The volume ratio of shark alkane reference substance and ethyl acetate is 1:5~20；
(2) prepared by sample solution：Saualane sample is taken, dissolving in ethyl acetate is added, sample solution, the saualane is made
The volume ratio of sample and ethyl acetate is 1:5~20；
(3) it measures：Saualane content in the sample solution obtained to step (2) using Gas chromatographyMass spectrometry into
Row measures, and GC conditions are：Chromatographic column：Stationary phase is the capillary column of -95% dimethyl polysiloxane of 5% phenyl, ruler
Very little is 30m × 0.25mm × 0.5 μm；Column temperature：150 DEG C of holding 4min, are warming up to 280 DEG C with the rate of 5~15 DEG C/min, keep
3min；Column flow rate：1.0mL/min；Injector temperature：250℃；Detector temperature：250℃；Carrier gas：Helium；Input mode：Point
Flow into sample, split ratio 5:1；Sample size：1 μ L, Mass Spectrometry Conditions are：EI ion source temperatures：230℃；Level four bars temperature：150℃；
Solvent delay 3min；Scan mode：SIM, it is 421 to select parent ion, daughter ion is respectively 29,43,57,71,85,99,113,
127、141、155、169、183、197、211、225、239、253、267、281、295、309、323、337、351、365、379、
393、407。
2. the assay method of saualane content according to claim 1, which is characterized in that the spiny dogfish described in step (1)
The volume ratio of alkane reference substance and ethyl acetate is 1:10.
3. the assay method of saualane content according to claim 1, which is characterized in that the spiny dogfish described in step (2)
The volume ratio of alkane sample and ethyl acetate is 1:10.
4. the assay method of saualane content according to claim 1, which is characterized in that the column temperature described in step (3)
For：150 DEG C of holding 4min, are warming up to 280 DEG C with the rate of 5 DEG C/min, keep 3min.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810242162.4A CN108593786B (en) | 2018-03-22 | 2018-03-22 | Method for measuring squalane content |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810242162.4A CN108593786B (en) | 2018-03-22 | 2018-03-22 | Method for measuring squalane content |
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| CN108593786A true CN108593786A (en) | 2018-09-28 |
| CN108593786B CN108593786B (en) | 2021-03-26 |
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| CN201810242162.4A Active CN108593786B (en) | 2018-03-22 | 2018-03-22 | Method for measuring squalane content |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109655541A (en) * | 2018-12-19 | 2019-04-19 | 汕头市中广测分析中心有限公司 | A kind of measuring method of tetradecylic acid content |
| CN114965778A (en) * | 2022-05-30 | 2022-08-30 | 江西威科油脂化学有限公司 | Method for determining palmitamide and stearamide in stearamide product |
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| JPH04305154A (en) * | 1990-06-08 | 1992-10-28 | Hitachi Cable Ltd | Capillary column for gas chromatography and manufacture thereof |
| CN102297916A (en) * | 2011-05-21 | 2011-12-28 | 太原理工大学 | Chromatograph apparatus for detecting sulfides in gas material, and detection method thereof |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109655541A (en) * | 2018-12-19 | 2019-04-19 | 汕头市中广测分析中心有限公司 | A kind of measuring method of tetradecylic acid content |
| CN114965778A (en) * | 2022-05-30 | 2022-08-30 | 江西威科油脂化学有限公司 | Method for determining palmitamide and stearamide in stearamide product |
| CN114965778B (en) * | 2022-05-30 | 2023-11-17 | 江西威科油脂化学有限公司 | Determination method of palmitoyl acid amide and stearic acid amide in stearic acid amide product |
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| CN108593786B (en) | 2021-03-26 |
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| CP02 | Change in the address of a patent holder | ||
| CP02 | Change in the address of a patent holder |
Address after: 515065 Room 05-2, Floor 10, Wantai Venture Building, No. 164, Mount Taishan North Road, Longhu District, Shantou City, Guangdong Province Patentee after: SHANTOU ZHONGGUANG TESTING AND ANALYSIS CENTER Co.,Ltd. Patentee after: Institute of testing and analysis, Guangdong Academy of Sciences (Guangzhou analysis and testing center, China) Address before: 515051 room 7b08-1, Jiesi information building, No. 6, Keji West Road, high tech Zone, Shantou City, Guangdong Province Patentee before: SHANTOU ZHONGGUANG TESTING AND ANALYSIS CENTER Co.,Ltd. Patentee before: Institute of testing and analysis, Guangdong Academy of Sciences (Guangzhou analysis and testing center, China) |