CN113325064A - Method for identifying charm peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry - Google Patents
Method for identifying charm peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry Download PDFInfo
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- CN113325064A CN113325064A CN202110595096.0A CN202110595096A CN113325064A CN 113325064 A CN113325064 A CN 113325064A CN 202110595096 A CN202110595096 A CN 202110595096A CN 113325064 A CN113325064 A CN 113325064A
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- atmospheric pressure
- emulsifier
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/62—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating the ionisation of gases, e.g. aerosols; by investigating electric discharges, e.g. emission of cathode
Abstract
The invention relates to the technical field of charm peak emulsifier ionization mass spectrometry identification, in particular to a method for identifying charm peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry, which specifically comprises five steps in order to solve the problem of higher requirements on sample pretreatment. The method omits a complicated sample pretreatment process, is simple to operate, short in extraction time, and quick, accurate and efficient in measurement, so that online detection can be conveniently realized, and meanwhile, a large amount of organic reagents are not required to be contacted, so that the harm to human body toxicity is solved, safety protection is increased, the atmospheric pressure chemical ionization mass spectrometry method is simple, convenient and efficient, and higher identification precision can be obtained for glamour peak emulsifier samples, so that the method can be applied to production in an expanded mode.
Description
Technical Field
The invention relates to the technical field of charm peak emulsifier ionization mass spectrum identification, in particular to a method for identifying charm peak emulsifier components by atmospheric pressure chemical ionization mass spectrum.
Background
Charm emulsifier is a natural, no polyethylene glycol, completely new O/W sensory emulsifier, with INCI names: polyglycerol-6 distearate (and) jojoba esters (and) polyglycerol-3 beeswax (and) cetyl alcohol, with a shiny milky appearance, a stealthy residual film and a smooth, pleasant after-feel. The charming emulsifier can be used for preparing light and thin emulsion or thick creamy cream, can be flexibly applied to skin care products and cosmetics with different textures, can automatically adapt to weather and seasons, can bring a very light and soft skin feeling to people, can keep moisture for a long time, and can improve the appearance of the skin. At present, the charm emulsifier is an innovative emulsifier mainly synthesized by polyglycerol fatty acid esters, no clear detection method is available about identification of the components of the emulsifier, and detection related to the polyglycerol fatty acid esters mainly adopts thin-layer chromatography, capillary chromatography, gas chromatography, supercritical fluid chromatography and high performance liquid chromatography, wherein the thin-layer chromatography, the capillary chromatography and the gas chromatography are relatively complex and long in time consumption, and the application of the methods is limited because a mixture cannot be well separated, so that the polyglycerol fatty acid esters are detected by the high performance liquid chromatography.
However, since high performance liquid chromatography requires high requirements for sample pretreatment, requires selection of a column and a mobile phase, and may be toxic to a human body by contacting a large amount of organic reagents, those skilled in the art have provided a method for identifying attractive peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry to solve the problems of the background art.
Disclosure of Invention
The invention aims to provide a method for identifying attractive peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry, which aims to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a method for identifying charm peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry comprises the following steps:
step 1: accurately weighing 100mg of sample, placing the sample in a 15mL glass centrifuge tube, adding 10mL ethyl acetate, heating to dissolve, cooling to room temperature, centrifuging, collecting supernatant of the glass centrifuge tube, and coating with a membrane;
step 2: an Atmospheric Pressure Chemical Ionization (APCI) ion source is adopted, the ion mode is a negative ion detection mode, the high pressure is 3000-3700V, and the temperature of a heating sleeve is 300-370 ℃;
and step 3: auxiliary spray N2Dry N at a pressure of 50-70 psi2The flow rate is 3-6L/min, and drying N2The temperature is 300-370 ℃;
and 4, step 4: injecting samples by using a flow injection pump at the flow rate of 100-800 mu L/min;
and 5: mass spectral profiles were recorded in full scan mode.
As a further aspect of the invention: the frequency of the centrifugation in the step 1 is 6000r/min, and the time is 10 min.
As a further aspect of the invention: the membrane filtration in step 1 was a 0.45 μm membrane.
As a further aspect of the invention: the high pressure in step 2 was 3500V.
As a further aspect of the invention: the heating jacket temperature described in step 2 was 350 ℃.
As a further aspect of the invention: auxiliary spraying N described in step 32The pressure was 60 psi.
As a further aspect of the invention: drying N in step 32The flow rate of (2) is 5L/min.
As a further aspect of the invention: drying N in step 32The temperature of (2) was 350 ℃.
As a further aspect of the invention: in the step 4, the sample injection flow rate is 500 mu L/min.
As a further aspect of the invention: the scanning quality range of the full scanning mode in the step 5 is m/z 100-1500.
Compared with the prior art, the invention has the beneficial effects that: the method omits a complicated sample pretreatment process, is simple to operate, short in extraction time, and quick, accurate and efficient in measurement, so that online detection can be conveniently realized, and meanwhile, a large amount of organic reagents are not required to be contacted, so that the harm to human body toxicity is solved, safety protection is increased, the atmospheric pressure chemical ionization mass spectrometry method is simple, convenient and efficient, and higher identification precision can be obtained for glamour peak emulsifier samples, so that the method can be applied to production in an expanded mode.
Drawings
FIG. 1 is a mass spectrum of the anion mode of an charm peak emulsifier sample 1 obtained in example 1;
FIG. 2 is a mass spectrum of negative ion mode m/z650-1150 of the charm peak emulsifier sample 1 of example 1;
FIG. 3 is a mass spectrum of the anion mode of the charm peak emulsifier sample 2 obtained in example 2;
FIG. 4 is a mass spectrum of the charm peak emulsifier sample 2 from example 2 in negative ion mode m/z 650-1150;
FIG. 5 is a mass spectrum of the negative ion mode of charm peak emulsifier sample 3 from example 3;
FIG. 6 is a mass spectrum of the negative ion mode m/z650-1150 of the obtained charm peak emulsifier sample 3;
FIG. 7 is a chemical structural formula spectrum of m/z 687;
FIG. 8 is a chemical structural formula spectrum of m/z 761;
FIG. 9 is a chemical structural formula diagram of m/z 999.
Detailed Description
Example 1
Referring to fig. 1-2, in an embodiment of the present invention, a method for identifying charming peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry includes the following steps:
step 1: accurately weighing 100mg of sample, placing the sample in a 15mL glass centrifuge tube, adding 10mL ethyl acetate, heating to dissolve, cooling to room temperature, centrifuging, collecting supernatant of the glass centrifuge tube, and coating with a membrane;
step 2: an Atmospheric Pressure Chemical Ionization (APCI) ion source is adopted, the ion mode is a negative ion detection mode, the high pressure is 3500V, and the temperature of a heating sleeve is 350 DEG C
And step 3: auxiliary spray N2Pressure 60psi, dry N2Flow rate of 5L/min, dry N2The temperature is 350 ℃;
and 4, step 4: adopting a flow injection pump to inject samples at the flow rate of 500 mu L/min;
and 5: mass spectral profiles were recorded in full scan mode.
Further, the frequency of the centrifugation in the step 1 is 6000r/min, and the time is 10 min.
Further, the membrane filtration in step 1 was a 0.45 μm filter.
Further, the scanning quality range of the full scanning mode in the step 5 is m/z 100-1500.
The experimental steps are as follows:
the instrument comprises the following steps: agilent Trap XCT ion Trap mass spectrometer
(1) Accurately weighing 100mg of sample 1, placing the sample in a 15mL glass centrifuge tube, adding 10mL ethyl acetate, heating to dissolve, cooling to room temperature, centrifuging at the rotating speed of 6000r/min for 10min, collecting supernatant, and filtering with a 0.45-micron filter membrane.
(2) And (3) adopting a flow injection pump for sample injection, wherein the sample injection flow rate is 500 mu L/min, recording a mass spectrum profile chart in a full scanning mode, and scanning the mass range m/z of 100-1500.
Example 2
Referring to fig. 3 to 4, a method for identifying charm peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry includes the following steps:
step 1: accurately weighing 100mg of sample, placing the sample in a 15mL glass centrifuge tube, adding 10mL ethyl acetate, heating to dissolve, cooling to room temperature, centrifuging, collecting supernatant of the glass centrifuge tube, and coating with a membrane;
step 2: an Atmospheric Pressure Chemical Ionization (APCI) ion source is adopted, the ion mode is a negative ion detection mode, the high pressure is 3000V, and the temperature of a heating sleeve is 300 ℃;
and step 3: auxiliary spray N2Pressure 50psi, dry N2Flow rate of 3L/min, dry N2The temperature is 300;
and 4, step 4: adopting a flow injection pump to inject samples at the flow rate of 100L/min;
and 5: mass spectral profiles were recorded in full scan mode.
Further, the frequency of the centrifugation in the step 1 is 6000r/min, and the time is 10 min.
Further, the membrane filtration in step 1 was a 0.45 μm filter.
Further, the scanning quality range of the full scanning mode in the step 5 is m/z 100-1500.
The experimental steps are as follows:
the instrument comprises the following steps: agilent Trap XCT ion Trap mass spectrometer
(1) Accurately weighing 100mg of sample 2, placing the sample 2 in a 15mL glass centrifuge tube, adding 10mL of ethyl acetate, heating to dissolve, cooling to room temperature, centrifuging at the rotating speed of 6000r/min for 10min, collecting supernatant, and filtering with a 0.45-micrometer filter membrane;
(2) and (3) adopting a flow injection pump for sample injection, wherein the flow rate of the sample injection is 100 mu L/min, recording a mass spectrum profile diagram in a full scanning mode, and scanning the mass range m/z of 100-1500.
Example 3
Referring to fig. 5 to 6, a method for identifying charm peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry includes the following steps:
step 1: accurately weighing 100mg of sample, placing the sample in a 15mL glass centrifuge tube, adding 10mL ethyl acetate, heating to dissolve, cooling to room temperature, centrifuging, collecting supernatant of the glass centrifuge tube, and coating with a membrane;
step 2: adopting an Atmospheric Pressure Chemical Ionization (APCI) ion source, wherein the ion mode is a negative ion detection mode, the high pressure is 3700V, and the heating sleeve temperature is 370 ℃;
and step 3: auxiliary spray N2Pressure 70psi, dry N2Flow rate of 6L/min, dry N2The temperature is 370 ℃;
and 4, step 4: adopting a flow injection pump to inject samples at the flow rate of 800 mu L/min;
and 5: mass spectral profiles were recorded in full scan mode.
Further, the frequency of the centrifugation in the step 1 is 6000r/min, and the time is 10 min.
Further, the membrane filtration in step 1 was a 0.45 μm filter.
Further, the scanning quality range of the full scanning mode in the step 5 is m/z 100-1500.
The experimental steps are as follows:
the instrument comprises the following steps: agilent Trap XCT ion Trap mass spectrometer
(1) Accurately weighing 100mg of sample 3, placing the sample in a 15mL glass centrifuge tube, adding 10mL ethyl acetate, heating to dissolve, cooling to room temperature, centrifuging at the rotating speed of 6000r/min for 10min, collecting supernatant, and filtering with a 0.45-micron filter membrane.
(2) And (3) adopting a flow injection pump for sample injection, wherein the sample injection flow rate is 800 mu L/min, recording a mass spectrum profile chart in a full scanning mode, and scanning the mass range m/z of 100-1500.
In summary, the following steps: as will be apparent from the description taken in conjunction with the accompanying figures 1 to 9: the method omits a complicated sample pretreatment process, is simple to operate, short in extraction time, and quick, accurate and efficient in measurement, so that online detection can be conveniently realized, and meanwhile, a large amount of organic reagents are not required to be contacted, so that the harm to human body toxicity is solved, safety protection is increased, the atmospheric pressure chemical ionization mass spectrometry method is simple, convenient and efficient, and higher identification precision can be obtained for glamour peak emulsifier samples, so that the method can be applied to production in an expanded mode.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention are equivalent to or changed within the technical scope of the present invention.
Claims (10)
1. A method for identifying attractive peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry is characterized by comprising the following steps:
step 1: accurately weighing 100mg of sample, placing the sample in a 15mL glass centrifuge tube, adding 10mL ethyl acetate, heating to dissolve, cooling to room temperature, centrifuging, collecting supernatant of the glass centrifuge tube, and coating with a membrane;
step 2: an Atmospheric Pressure Chemical Ionization (APCI) ion source is adopted, the ion mode is a negative ion detection mode, the high pressure is 3000-3700V, and the temperature of a heating sleeve is 300-370 ℃;
and step 3: auxiliary spray N2Dry N at a pressure of 50-70 psi2The flow rate is 3-6L/min, and drying N2The temperature is 300-370 ℃;
and 4, step 4: injecting samples by using a flow injection pump at the flow rate of 100-800 mu L/min;
and 5: mass spectral profiles were recorded in full scan mode.
2. The method for identifying the composition of an attractive peak emulsifier by atmospheric pressure chemical ionization mass spectrometry as claimed in claim 1, wherein the frequency of the centrifugation in step 1 is 6000r/min, and the time is 10 min.
3. The method for identifying the composition of an attractive peak emulsifier by atmospheric pressure chemical ionization mass spectrometry as claimed in claim 1, wherein the membrane used in step 1 is a 0.45 μm filter membrane.
4. The method for identifying attractive peak emulsifier components by atmospheric pressure chemical ionization mass spectrometry as claimed in claim 1, wherein the high pressure in step 2 is 3500V.
5. The method of claim 1 wherein the heating jacket temperature of step 2 is 350 ℃.
6. The method for identifying attractive peak emulsifier composition by atmospheric pressure chemical ionization mass spectrometry as claimed in claim 1, wherein the auxiliary spray N in step 32The pressure was 60 psi.
7. The method of claim 1, wherein the drying step 3 is performed in the presence of dry N2The flow rate of (2) is 5L/min.
8. The method of claim 1, wherein the drying step 3 is performed in the presence of dry N2The temperature of (2) was 350 ℃.
9. The method for identifying the composition of an attractive peak emulsifier by atmospheric pressure chemical ionization mass spectrometry as claimed in claim 1, wherein the flow rate of the sample injection in step 4 is 500 μ L/min.
10. The method of claim 1, wherein the scanning mass range of the full scan mode in step 5 is m/z 100-1500.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001249114A (en) * | 1999-12-27 | 2001-09-14 | Hitachi Ltd | Mass spectrometry and mass spectrometer |
| US20030207460A1 (en) * | 2002-01-25 | 2003-11-06 | Ciphergen Biosystems, Inc. | Monomers and polymers having energy absorbing moieties of use in desorption/ionization of analytes |
| CN1717381A (en) * | 2002-11-28 | 2006-01-04 | 大赛璐化学工业株式会社 | Polyglycerols, polyglycerol/fatty acid ester, and processes for producing these |
| US20060292246A1 (en) * | 2005-06-20 | 2006-12-28 | Rey-Yuh Wu | Characteristic mass spectral fingerprint setting method and rapid identification method for Chinese herbal medicines and prescriptions |
| US20180120327A1 (en) * | 2015-03-12 | 2018-05-03 | Mars, Incorporated | Ultra high resolution mass spectrometry and methods of using the same |
| CN112014497A (en) * | 2020-08-20 | 2020-12-01 | 南昌大学 | Method for simultaneously detecting three monoglyceride emulsifiers in dairy product based on gas chromatography-mass spectrometry |
-
2021
- 2021-05-28 CN CN202110595096.0A patent/CN113325064A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001249114A (en) * | 1999-12-27 | 2001-09-14 | Hitachi Ltd | Mass spectrometry and mass spectrometer |
| US20030207460A1 (en) * | 2002-01-25 | 2003-11-06 | Ciphergen Biosystems, Inc. | Monomers and polymers having energy absorbing moieties of use in desorption/ionization of analytes |
| CN1717381A (en) * | 2002-11-28 | 2006-01-04 | 大赛璐化学工业株式会社 | Polyglycerols, polyglycerol/fatty acid ester, and processes for producing these |
| US20060292246A1 (en) * | 2005-06-20 | 2006-12-28 | Rey-Yuh Wu | Characteristic mass spectral fingerprint setting method and rapid identification method for Chinese herbal medicines and prescriptions |
| US20180120327A1 (en) * | 2015-03-12 | 2018-05-03 | Mars, Incorporated | Ultra high resolution mass spectrometry and methods of using the same |
| CN112014497A (en) * | 2020-08-20 | 2020-12-01 | 南昌大学 | Method for simultaneously detecting three monoglyceride emulsifiers in dairy product based on gas chromatography-mass spectrometry |
Non-Patent Citations (4)
| Title |
|---|
| M. CORTESE ET AL.: "Qualitative characterization of a transesterification product of coconut oil by FIA-APCI-MS", 《INTERNATIONAL JOURNAL OF COSMETIC SCIENCE》 * |
| WM. CRAIG BYRDWELL ET AL.: "Quantitative Analysis of Triglycerides Using Atmospheric Pressure Chemical Ionization-Mass Spectrometry", 《LIPIDS》 * |
| 杨继生 等: "脂肪酸聚甘油酯的分析", 《食品科学》 * |
| 闫峻 等: "复方板蓝根颗粒ACPI-MS指纹图谱及化学成分的LC-APCI-MSn研究", 《质谱学报》 * |
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Application publication date: 20210831 |