CN112924585A - Qualitative analysis method of linear dimethyl siloxane in polydimethylsiloxane - Google Patents
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- 239000004205 dimethyl polysiloxane Substances 0.000 title claims abstract description 52
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 title claims abstract description 52
- -1 dimethyl siloxane Chemical class 0.000 title claims abstract description 51
- 238000004451 qualitative analysis Methods 0.000 title claims abstract description 30
- 238000000034 method Methods 0.000 title claims abstract description 25
- 238000001819 mass spectrum Methods 0.000 claims abstract description 27
- 238000001228 spectrum Methods 0.000 claims abstract description 4
- 235000013870 dimethyl polysiloxane Nutrition 0.000 claims abstract 13
- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 claims abstract 7
- 238000004987 plasma desorption mass spectroscopy Methods 0.000 claims abstract 7
- 238000000065 atmospheric pressure chemical ionisation Methods 0.000 claims description 8
- 230000003595 spectral effect Effects 0.000 claims description 7
- 239000012159 carrier gas Substances 0.000 claims description 4
- 239000001307 helium Substances 0.000 claims description 4
- 229910052734 helium Inorganic materials 0.000 claims description 4
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 claims description 4
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- 238000004458 analytical method Methods 0.000 abstract description 8
- 238000004949 mass spectrometry Methods 0.000 abstract description 3
- 150000002500 ions Chemical group 0.000 description 14
- 238000002451 electron ionisation mass spectrometry Methods 0.000 description 10
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 5
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- 238000002347 injection Methods 0.000 description 4
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- 230000014759 maintenance of location Effects 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- 239000012491 analyte Substances 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 238000000605 extraction Methods 0.000 description 2
- 239000007789 gas Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000282414 Homo sapiens Species 0.000 description 1
- 206010067572 Oestrogenic effect Diseases 0.000 description 1
- 239000012298 atmosphere Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 231100000693 bioaccumulation Toxicity 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 150000001793 charged compounds Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- FBZANXDWQAVSTQ-UHFFFAOYSA-N dodecamethylpentasiloxane Chemical group C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C FBZANXDWQAVSTQ-UHFFFAOYSA-N 0.000 description 1
- 229940087203 dodecamethylpentasiloxane Drugs 0.000 description 1
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- 238000013467 fragmentation Methods 0.000 description 1
- 238000006062 fragmentation reaction Methods 0.000 description 1
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- NFVSFLUJRHRSJG-UHFFFAOYSA-N hexadecamethylheptasiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C NFVSFLUJRHRSJG-UHFFFAOYSA-N 0.000 description 1
- 238000004896 high resolution mass spectrometry Methods 0.000 description 1
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- 238000004445 quantitative analysis Methods 0.000 description 1
- JEULYRSRLMIJQJ-UHFFFAOYSA-N silyloxy(tetradecylsilyloxysilyloxysilyloxysilyloxy)silane Chemical compound C(CCCCCCCCCCCCC)[SiH2]O[SiH2]O[SiH2]O[SiH2]O[SiH2]O[SiH3] JEULYRSRLMIJQJ-UHFFFAOYSA-N 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- KJBTUARYMVBZAE-UHFFFAOYSA-N trimethyl(trimethylsilyloxysilyloxysilyloxysilyloxysilyloxysilyloxy)silane Chemical compound C[Si](O[SiH2]O[SiH2]O[SiH2]O[SiH2]O[SiH2]O[Si](C)(C)C)(C)C KJBTUARYMVBZAE-UHFFFAOYSA-N 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
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- G01N30/02—Column chromatography
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- G01N30/86—Signal analysis
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Abstract
The invention discloses a qualitative analysis method of linear dimethyl siloxane in polydimethylsiloxane. The invention utilizes GC-APCI-QtofMS to analyze a PDMS (5vSt) sample, and then uses an elementalComplexion tool in Masslynx to perform fitting analysis on the mass spectrum result corresponding to each spectrum peak to give a corresponding qualitative result. The method for qualitatively analyzing the linear dimethyl siloxane in the PDMS based on the soft ionization mass spectrometry is accurate and sensitive, and can solve the problem that the qualitative analysis of the linear dimethyl siloxane in the PDMS is inaccurate at present.
Description
Technical Field
The invention relates to the technical field of analytical chemistry, in particular to a qualitative analysis method of linear dimethyl siloxane in polydimethylsiloxane.
Background
Dimethyl siloxanes (dimethylsiloxanes) are widely used in daily life and industry because of their excellent physicochemical properties. Dimethyl siloxane is continuously introduced into the environment along with the activities of human beings, and is found in the environment media such as atmosphere, soil, water, dust particles and the like, and researches show that the content of linear methyl siloxane is up to 42800 ng/g. In addition, dimethyl siloxane has been found to have persistence, long-range migration properties, bioaccumulation, and potential toxic and estrogenic effects, and thus is identified as an "emerging pollutant" and is of great interest.
Dimethylsiloxanes of interest for environmental health studies include cyclic dimethylsiloxanes (Dn (n is the number of silicon atoms, n.gtoreq.3)) and linear dimethylsiloxanes (Ln (n is the number of silicon atoms, n.gtoreq.2)). As the cyclic dimethyl siloxane has a single standard substance, the cyclic dimethyl siloxane can be accurately analyzed and detected when being subjected to qualitative and quantitative analysis; while the partial linear dimethyl siloxane (especially with molecular weight more than 600Da, n is more than or equal to 7) is difficult to separate out a single component with high purity meeting the standard due to the special property, when the pollutants are researched, Polydimethylsiloxane (PDMS) is usually adopted as a standard sample (PDMS (5vSt)), so the qualitative analysis of the linear monomer dimethyl siloxane (Ln, more than or equal to 7) component in PDMS is particularly important before the PDMS is used; the accuracy of qualitative analysis of components in the PDMS standard sample determines whether a series of subsequent research results about environmental monitoring, ecological risks, health and the like are reliable and accurate.
At present, a qualitative analysis method for linear dimethylsiloxane components in PDMS is to adopt GC-EI-MS to obtain a mass spectrum under a scan (full scan) mode, compare the mass spectrum with a mass spectrum of a known single linear siloxane, and further estimate the linear dimethylsiloxane components in PDMS according to whether the linear dimethylsiloxane components contain the same ion fragments or not. However, the capillary chromatographic column of the GC system has a large component of methyl siloxane column loss, the column loss in the EI ion source (electron bombardment ion source) also forms the same ion fragments as linear dimethyl siloxane, and the qualitative determination of the linear dimethyl siloxane component in PDMS by comparing the qualitative determination of whether the mass spectrum contains the same ion fragments is obviously not suitable and accurate. This qualitative analysis method by "guess" method brings about great deviation and even gives wrong results. The reason for this is that in the EI ion source, molecules of the analyte are given too much internal energy, resulting in continuous fragmentation of the molecules after ionization, making it difficult to determine the molecular weight of the analyte, and also making it impossible to search for unknown substances using the electron ionization spectrum library, resulting in inaccurate qualitative analysis. Therefore, a technical solution capable of solving the problem of inaccurate qualitative analysis of linear dimethylsiloxane in PDMS is needed.
Disclosure of Invention
The invention aims to provide a qualitative analysis method of linear dimethyl siloxane in Polydimethylsiloxane (PDMS), which adopts a gas-time-of-flight mass spectrometer (GC-APCI-QtofMS) to qualitatively analyze linear dimethyl siloxane components in PDMS so as to solve the problem that the current qualitative analysis of linear dimethyl siloxane in PDMS is inaccurate.
In order to achieve the purpose, the invention provides the following technical scheme:
the qualitative analysis method of the linear dimethyl siloxane in the PDMS is provided, and comprises the following steps:
(1) preparing a sample of PDMS (5 vSt);
(2) PDMS (5vSt) samples were analyzed using GC-APCI-QtofMS;
(3) and (4) carrying out qualitative analysis on mass spectrum results corresponding to the various spectral peaks measured by GC-APCI-QtofMS.
Preferably, the mass spectrum results corresponding to each spectrum peak measured by GC-APCI-QtofMS are subjected to fitting analysis by using an element Composition tool in Masslynx to give corresponding qualitative results.
Preferably, the concentration of the PDMS (5vSt) sample in step (1) is 10 mg/L.
Preferably, the chromatographic conditions for analyzing the PDMS (5vSt) sample using GC-APCI-QtofMS in step (2) are:
a chromatographic column: DB5-MS column with specification of 30m × 0.25mm × 0.25 μm;
temperature programming: keeping the temperature at 40 ℃ for 2min, increasing the temperature to 220 ℃ at the speed of 20 ℃/min, increasing the temperature to 290 ℃ at the speed of 5 ℃/min, keeping the temperature for 5min, keeping the temperature of a transmission line at 300 ℃,
and (3) sample introduction mode: no shunt sample introduction, and helium as carrier gas;
an ion source: atmospheric pressure chemical ionization source (APCI), ion source temperature 150 ℃;
ionization mode: APGC+A mode;
gas circuit: the air flow rate of the taper hole is 150L/h, and the auxiliary air flow rate is 200L/h;
the scanning mode is as follows: the Mass spectrum was scanned in MS Scan (i.e. Full Scan) mode and the Mass spectrum results corresponding to each spectral peak were corrected with Lock Mass.
Preferably, the amount of the non-split sample is 1. mu.L.
Preferably, the Scan range of the Scan mode is 100-1500 m/z.
Preferably, the Lock Mass set value is 281.0517 m/z.
In APCI ion source, target molecule is ionized to generate excimer ions ([ M + H ]]+) Can be detected.
The invention has the following beneficial technical effects:
the invention utilizes a GC-APCI-QtofMS analysis method to carry out qualitative analysis on linear dimethyl siloxane in PDMS, and is atmospheric pressure chemical ionization based on soft ionization technologyIon source (APCI), in the case of ionizing the target, forms molecular ions (M +), excimer ions ([ M + H ]), which can indicate "molecular characteristics]+，[M+Na]+Etc.), which can be readily and accurately resolved in high resolution mass spectrometry, can be used for accurate characterization of unknown analytes.
The qualitative analysis method for linear dimethyl siloxane in PDMS disclosed by the invention is accurate and sensitive, has low detection concentration, and can solve the problem that the qualitative analysis of linear dimethyl siloxane in PDMS is inaccurate at present.
Drawings
FIG. 1 is a graph obtained by testing PDMS (5vSt) by GC-APCI-QtofMS in example 1; wherein FIG. 1(a) is a mass extraction chromatogram; FIG. 1(b) is a mass spectrum corresponding to L17; FIG. 1(c) shows a mass spectrum corresponding to L18.
FIG. 2 is a gas chromatogram obtained by detecting PDMS (5vSt) by GC-EI-MS in comparative example 1.
FIG. 3 is a mass spectrum of PDMS (5vSt) detected by GC-EI-MS in comparative example 1.
FIG. 4 is a mass spectrum of PDMS (5vSt) detected by GC-EI-MS in comparative example 1.
Detailed Description
Reference will now be made in detail to various exemplary embodiments of the present invention, examples of which are illustrated in the accompanying drawings, and this detailed description should not be taken to be limiting of the invention, but is rather a more detailed description of certain aspects, features and embodiments of the invention. It is to be understood that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Further, for numerical ranges in this disclosure, it is understood that each intervening value, between the upper and lower limit of that range, is also specifically disclosed. Every smaller range between any stated value or intervening value in a stated range and any other stated or intervening value in a stated range is encompassed within the invention. The upper and lower limits of these smaller ranges may independently be included or excluded in the range.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. Although only preferred methods and materials are described herein, any methods and materials similar or equivalent to those described herein can be used in the practice or testing of the present invention.
As used herein, the terms "comprising," "including," "having," "containing," and the like are open-ended terms that mean including, but not limited to.
Example 1
(1) PDMS (5vSt) sample was prepared
1.0mg of PDMS (5vSt) standard sample is weighed and dissolved in 1000 mul of n-hexane to prepare a mother solution with the concentration of 1000mg/L, and then the mother solution is diluted by n-hexane to obtain a sample to be tested with the concentration of 10 mg/L.
(2) GC-APCI-QtofMS qualitative analysis of PDMS (5vSt) samples
GC-APCI-QtofMS analysis conditions: DB5-MS column (30m × 0.25mm × 0.25 μm), temperature programmed:
keeping for 5min, conveying line temperature 300 deg.C, no split-flow sample injection, helium as carrier gas, and sample injection amount of 1 μ L. The ion source is an atmospheric pressure chemical ionization source (APCI), and the ionization mode is APGC+150L/h of taper hole airflow speed, 200L/h of auxiliary airflow speed, 150 ℃ of ion source temperature, a Mass spectrum adopting an MS Scan (namely Full Scan) mode, a scanning range of 100-1500m/z, a Lock Mass: 281.0517 (column run off).
Detecting and analyzing a 10mg/L PDMS (5vSt) standard sample by GC-APCI-QtofMS, and performing isotope mass extraction to obtain fourteen chromatographic peaks shown in figure 1(a), wherein figure 1(b) is a mass spectrum corresponding to L17, and figure 1(c) is a mass spectrum corresponding to L18. The mass spectrum results corresponding to the individual chromatographic peaks were qualitatively analyzed using the elementary Composition tool of massynx, and the analysis results are detailed in table 1.
TABLE 1
Note that mDa represents the deviation between the actual detection Mass and the theoretical calculation Mass of the target Mass spectrum, and the absolute value allowable range is less than or equal to 5.0; PPM represents the relative deviation between the actual detection Mass and the theoretical calculation Mass of the target Mass spectrum, and the absolute value allowable range is less than or equal to 10.0.
Comparative example 1
(1) PDMS (5vSt) samples were prepared:
1.0mg of PDMS (5vSt) standard sample is weighed and dissolved in 1000 mul of n-hexane to prepare a mother solution with the concentration of 1000mg/L, and then the mother solution is diluted by the n-hexane to prepare a sample to be tested with the concentration of 300 mg/L.
(2) GC-EI-MS qualitative analysis of PDMS (5vSt) samples
GC-EI-MS analysis conditions: HP-5MS column (30 m.times.0.25 mm.times.0.25 μm), temperature programmed:
keeping for 5min, conveying line temperature 300 deg.C, no split-flow sample injection, helium as carrier gas, and sample injection amount of 1 μ L. The ion source is an electron impact source (EI), the adopted mode is a Full Scan mode, and the mass spectrum scanning range is 50-600 m/z.
The detection analysis of 300mg/L PDMS (5vSt) standard sample by GC-EI-MS detects fourteen dominant peaks as shown in FIG. 2, and the retention time is 8.320min, 9.492min, 10.522min, 11.456min, 12.463min, 13.637min, 15.033min, 16.635min, 18.380min, 20.208min, 22.041min, 23.834min, 25.608min and 27.716 min. The mass spectrograms corresponding to the fourteen dominant chromatographic peaks are shown in fig. 3 and fig. 4, and fig. 3 is the mass spectrograms corresponding to retention times of 8.320min, 9.492min, 10.522min, 11.456min, 12.463min, 13.637min and 15.033min in sequence from top to bottom; FIG. 4 is a mass spectrum diagram with retention times of 16.635min, 18.380min, 20.208min, 22.041min, 23.834min, 25.608min and 27.716min in sequence from top to bottom. Wherein the chromatographic peak corresponding to 8.320min is searched with NIST spectral library, and the matching result is dodecamethylpentasiloxane (L5, C)12H36O4Si5) The matching degree is 91.6%; 9.492min chromatogram peak retrieval gave tetradecyl hexasiloxane (L6, C)14H42O5Si6) The matching degree is 98.1%; 10.522min peak search gave Hexamethylheptasiloxane (L7, C)16H48O6Si7) The degree of matching was 98.3%. The rest chromatographic peaks have no accurate retrieval result in the NIST spectral library. Comparing the mass spectra corresponding to the fourteen dominant chromatographic peaks, it can be found that the mass spectra fragments corresponding to different chromatographic peaks are not very different, and from the fourth chromatographic peak (11.456min), the results matched by NIST spectral library search are all hexadecamethylheptasiloxane (L7, C7)16H48O6Si7) That is, the accurate qualitative analysis of the subsequent chromatographic peak cannot be performed.
By comparing the analysis results of the example 1(GC-APCI-QtofMS qualitative analysis method) and the comparative example 1(GC-EI-MS qualitative analysis method), the qualitative method of linear dimethyl siloxane in PDMS based on soft ionization mass spectrometry provided by the invention can accurately and qualitatively analyze three single dimethyl siloxanes L5, L6 and L7 determined by GC-EI-MS qualitative analysis under lower concentration, and can also provide qualitative results corresponding to other eleven chromatographic peaks, so that the qualitative method of linear dimethyl siloxane in PDMS based on soft ionization mass spectrometry is more accurate and sensitive compared with the traditional GC-EI-MS qualitative analysis method.
The above-described embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements of the technical solutions of the present invention can be made by those skilled in the art without departing from the spirit of the present invention, and the technical solutions of the present invention are within the scope of the present invention defined by the claims.
Claims (7)
1. A qualitative analysis method for linear dimethyl siloxane in polydimethylsiloxane is characterized by comprising the following steps:
(1) preparing a sample of PDMS (5 vSt);
(2) PDMS (5vSt) samples were analyzed using GC-APCI-QtofMS;
(3) and (4) carrying out qualitative analysis on mass spectrum results corresponding to the various spectral peaks measured by GC-APCI-QtofMS.
2. The method of claim 1, wherein the qualitative analysis of linear dimethylsiloxane in polydimethylsiloxane is performed by fitting and analyzing the mass spectrum results corresponding to each spectrum peak measured by GC-APCI-QtofMS using an element Composition tool in Masslynx to give the corresponding qualitative results.
3. The method of qualitative analysis of linear dimethylsiloxane in polydimethylsiloxane according to claim 1, wherein the concentration of the PDMS (5vSt) sample in step (1) is 10 mg/L.
4. The method for qualitatively analyzing linear dimethylsiloxane in polydimethylsiloxane of claim 1, wherein the chromatographic conditions for analyzing the PDMS (5vSt) sample by GC-APCI-QtofMS in the step (2) are as follows:
a chromatographic column: DB5-MS column with specification of 30m × 0.25mm × 0.25 μm;
temperature programming: maintaining at 40 deg.C for 2min, increasing to 220 deg.C at 20 deg.C/min, increasing to 290 deg.C at 5 deg.C/min, maintaining for 5min, and maintaining at transmission line temperature of 300 deg.C;
and (3) sample introduction mode: no shunt sample introduction, and helium as carrier gas;
an ion source: an atmospheric pressure chemical ionization source;
ionization mode: APGC+In the mode, the air flow rate of the taper hole is 150L/h, the auxiliary air flow rate is 200L/h, and the ion source temperature is 150 ℃;
the scanning mode is as follows: the Mass spectrum is scanned by adopting an MS Scan mode, and Mass spectrum results corresponding to various spectral peaks are corrected by using Lock Mass.
5. The method of claim 4, wherein the amount of the undivided sample is 1 μ L.
6. The method as claimed in claim 4, wherein the MS Scan mode is performed in a scanning range of 100-1500 m/z.
7. The method for qualitatively analyzing linear dimethylsiloxane in polydimethylsiloxane according to claim 4, wherein the Lock Mass set value is 281.0517 m/z.
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| CN106568867A (en) * | 2016-10-31 | 2017-04-19 | 河南师范大学 | Quantitative method of chain-like methylsiloxane in PDMS |
| CN111929384A (en) * | 2020-07-31 | 2020-11-13 | 淄博鲁瑞精细化工有限公司 | Method for determining content of residual methyl siloxane in organic silicon softening agent by using HS-GC external standard method |
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