CN105067739A - Laurinol polyoxyethylene ether fully two-dimensional separation analysis method - Google Patents

Laurinol polyoxyethylene ether fully two-dimensional separation analysis method Download PDF

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CN105067739A
CN105067739A CN201510450876.0A CN201510450876A CN105067739A CN 105067739 A CN105067739 A CN 105067739A CN 201510450876 A CN201510450876 A CN 201510450876A CN 105067739 A CN105067739 A CN 105067739A
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dodecyl alcohol
ethoxylated dodecyl
dimensional separation
full
ionic mobility
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马强
白桦
孟宪双
郭项雨
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Chinese Academy of Inspection and Quarantine CAIQ
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Chinese Academy of Inspection and Quarantine CAIQ
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Abstract

The invention discloses a laurinol polyoxyethylene ether fully two-dimensional separation analysis method including the following steps: an ultrahigh pressure hydrophilic interaction chromatography-ion mobility mass spectrometry coupled method is adopted, a laurinol polyoxyethylene ether fully two-dimensional separation analysis system is constructed, and effective separation and accurate determination of a complex target compound system are realized; the method includes optimization of ultrahigh hydrophilic interaction chromatography conditions and ion mobility mass spectrometry conditions. According to the laurinol polyoxyethylene ether fully two-dimensional separation analysis method, through the ultrahigh pressure hydrophilic interaction chromatography-ion mobility mass spectrometry coupling technique, the laurinol polyoxyethylene ether fully two-dimensional separation analysis method is developed, and rapid separation detection of laurinol polyoxyethylene ether is realized.

Description

A kind of full two dimensional separation analytical approach of ethoxylated dodecyl alcohol
Technical field
The present invention relates to a kind of full two dimensional separation analytical approach of chemical substance, particularly relate to the full two dimensional separation analytical approach of ethoxylated dodecyl alcohol.
Background technology
Ethoxylated dodecyl alcohol belongs to a kind of important AEO, is one of with fastest developing speed in non-ionic surfactant, that consumption is maximum kind.Ehter bond in molecule is not easily destroyed by acid, alkali, so stability is higher, better water-soluble, electrolyte-resistant, is easy to biodegradation, and foam is little.Except using in a large number in textile printing and dyeing industry, also a large amount of for composite low sudsing liquid detergent.The compatibility of ethoxylated dodecyl alcohol and other surfactants is good.Insensitive to hard water, cold washing performance is good, but along with the rising of water temperature, its solubleness can reduce gradually.In the scope that pH value is 3 ~ 11, ethoxylated dodecyl alcohol hydrolysis-stable.But they also can slow oxidation in atmosphere, and produce some oxidation products, such as acetaldehyde and hydroperoxides, the surfactant that these oxides, than those, analogue not yet occur is larger to dermal toxicity.Be mainly used in washing industry, textile printing and dyeing industry, paper industry.The ethoxylated dodecyl alcohol chemical risk material that can contain in the sample such as product, ecologic environment, all can produce human cancer cell's growth and fecundity and have a strong impact on, all form serious harm to health and ecologic environment.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of full two dimensional separation analytical approach of ethoxylated dodecyl alcohol.
A kind of full two dimensional separation analytical approach of ethoxylated dodecyl alcohol, adopt the method for the hydrophilic interaction chromatography of UHV (ultra-high voltage) and ionic mobility mass spectrometry, construct the full two dimensional separation analysis system of ethoxylated dodecyl alcohol, achieve effective separation and the precise determination of complex target compound system, described method comprises the optimization of UHV (ultra-high voltage) aqueous favoring interaction chromatographic condition and ionic mobility Mass Spectrometry Conditions.
The full two dimensional separation analytical approach of ethoxylated dodecyl alcohol of the present invention, wherein said UHV (ultra-high voltage) aqueous favoring interaction chromatographic condition is as follows:
(1) chromatographic column: WatersACQUITYUPLCHSSHILIC post, 100mm × 2.1mm, 1.8 μm;
(2) mobile phase: water-acetonihile gradient elution, gradient elution program is in table 1;
(3) flow velocity: 0.4mL/min;
(4) column temperature: 35 DEG C;
(5) sample chamber temperature: 10 DEG C;
(6) sample size: 10 μ L;
(7) pin liquid is washed: washing by force pin liquid is water, 200 μ L; Weak pin liquid of washing is acetonitrile, 600 μ L.
Table 1 gradient elution program
The full two dimensional separation analytical approach of ethoxylated dodecyl alcohol of the present invention, wherein said ionic mobility Mass Spectrometry Conditions is as follows:
(1) ion gun: electron spray ionisation source;
(2) scan mode: positive ion mode;
(3) capillary voltage: 2.8kV;
(4) desolventizing temperature degree: 500 DEG C;
(5) desolventizing airshed: 1000L/h;
(6) taper hole voltage is sampled: 65V;
(7) taper hole voltage is extracted: 4.0V;
(8) trap ions inducting device collision energy: 6.0V;
(9) trap ions inducting device flow: 1.5mL/min;
(10) mobility wave speed: 700m/sec;
(11) mobility wave height: 40V;
(12) mobility gas velocity: 90mL/min;
(13) flight time mass spectrum mass analyzer quality acquisition range: m/z50to1500Da;
(14) flight time mass spectrum mass analyzer sweep time: 1.0sec;
(15) flight time mass spectrum mass analyzer sweep interval: 0.02sec;
(16) lock mass number reference corrected liquid: LEK solution, 200ng/mL, m/z556.2771Da.
The full two dimensional separation analytical approach of ethoxylated dodecyl alcohol of the present invention, wherein said method also comprises the long-pending computing method of ethoxylated dodecyl alcohol collision cross section, described computing method comprise the steps: to select polyalanine to be calibration substance, with the known collision cross section product value of described polyalanine to ionic mobility transit time, draw single electric charge, double charge and tricharged three calibration curves respectively; And then, under identical experiment condition, ethoxylated dodecyl alcohol is tested, according to the calibrating curve equation released with polyalanine, extrapolate the collision cross section product value of ethoxylated dodecyl alcohol monomer of different electric charge, different polymerization degree.
The full two dimensional separation analytical approach difference from prior art of ethoxylated dodecyl alcohol of the present invention is: the full two dimensional separation analytical approach of ethoxylated dodecyl alcohol of the present invention, by the hydrophilic interaction chromatography of UHV (ultra-high voltage) and the mass spectrographic coupling technique of ionic mobility, develops the full two dimensional separation analytical approach of ethoxylated dodecyl alcohol.Ionic mobility completes the rear ionization quick separating of target compound in 6.4ms.Carry the difference of ethoxylated dodecyl alcohol according to ionic mobility of single electric charge, double charge and tricharged, can realize being separated.By the hydrophilic interaction chromatography of UHV (ultra-high voltage) and the mass spectrographic conbined usage of ionic mobility, target substance can be separated with ionic mobility based on hydrophobicity simultaneously.The constructed hydrophilic interaction chromatography of the UHV (ultra-high voltage)-orthogonality related coefficient of the full two-dimensional system of ionic mobility mass spectrum to ethoxylated dodecyl alcohol is 0.0224, and peak dispersion angle is 88.72 °.The actual peak capacity of this full two dimensional separation analysis system reaches 7713, is 40 times and 193 times that are used alone the first dimension separation and two dimensional separation respectively.Also calculated the collision cross section product value of ethoxylated dodecyl alcohol of different polymerization degree, different electric charge simultaneously.
Be described further below in conjunction with the full two dimensional separation analytical approach of accompanying drawing to ethoxylated dodecyl alcohol of the present invention.
Accompanying drawing explanation
Fig. 1 is the total ion current figure that in the present invention, the hydrophilic interaction chromatography of UHV (ultra-high voltage) is separated with ionic mobility; Wherein, Fig. 1 a is the UHV (ultra-high voltage) aqueous favoring interaction chromatographic resolution total ion current figure of ethoxylated dodecyl alcohol, and Fig. 1 b, Fig. 1 c, Fig. 1 d are respectively the ionic mobility separating spectrum of the ethoxylated dodecyl alcohol with single electric charge, double charge and tricharged; The degree of polymerization of the corresponding ethoxylated dodecyl alcohol of institute's reference numbers on each chromatographic peak or ionic mobility peak in Fig. 1;
Fig. 2 is full scan mass spectrogram in the present invention; Wherein, Fig. 2 a is the full scan mass spectrogram that ethoxylated dodecyl alcohol is separated without ionic mobility; Fig. 2 b, Fig. 2 c, Fig. 2 d are respectively the full scan mass spectrogram of single electric charge, double charge and the tricharged of ethoxylated dodecyl alcohol after ionic mobility separation, background correction;
Fig. 3 is the UHV (ultra-high voltage) of ethoxylated dodecyl alcohol in the present invention hydrophilic mutual chromatographic retention figure and ionic mobility transit time figure; Wherein, Fig. 3 a is the ionic mobility transit time-UHV (ultra-high voltage) aqueous favoring interaction chromatographic retention figure of ethoxylated dodecyl alcohol; Fig. 3 b is the mass-to-charge ratio-UHV (ultra-high voltage) aqueous favoring interaction chromatographic retention figure of ethoxylated dodecyl alcohol; Fig. 3 c is the mass-to-charge ratio-ionic mobility transit time figure of ethoxylated dodecyl alcohol;
Fig. 4 is the mass-to-charge ratio-ionic mobility transit time figure of polyalanine in the present invention;
Fig. 5 is the polyalanine calibration curve carrying single electric charge, double charge and tricharged in the present invention.
The corresponding translator of Chinese of the English related in institute's drawings attached is as follows:
RelativeAbundance: relative abundance; RetentionTime: retention time; DriftTime: transit time; M/z: mass-to-charge ratio; CCS: collision cross section amasss: SinglyCharged: carry single electric charge; DoublyCharged: carry double charge; TriplyCharged: carry tricharged; R 2: related coefficient.
Embodiment
Embodiment 1
One, instrument and reagent
ACQUITY Ultra Performance Liquid Chromatography instrument, be furnished with binary pump, sample manager, column oven, SYNAPTG2-SiHDMS quadrupole rod-ionic mobility-flight time tandem mass spectrometer, MassLynx and DriftScope data handling system (Waters, US); Mixed sample ethoxylated dodecyl alcohol (average degree of polymerization is 23) purchased from American ChemService company.Acetonitrile is chromatographically pure (J.T.Baker company of the U.S.); Water is ultrapure water prepared by Milli-Q Superpure water machine (Millipore company of the U.S.).
Two, experimental technique
1, UHV (ultra-high voltage) aqueous favoring interaction chromatographic condition
(1) chromatographic column: WatersACQUITYUPLCHSSHILIC post (100mm × 2.1mm, 1.8 μm);
(2) mobile phase: water-acetonihile gradient elution (gradient elution program is in table 1);
(3) flow velocity: 0.4mL/min;
(4) column temperature: 35 DEG C;
(5) sample chamber temperature: 10 DEG C;
(6) sample size: 10 μ L;
(7) pin liquid is washed: washing by force pin liquid is water, 200 μ L; Weak pin liquid of washing is acetonitrile, 600 μ L.
Table 1 gradient elution program
2, ionic mobility Mass Spectrometry Conditions
(1) ion gun: electron spray ionisation source;
(2) scan mode: positive ion mode;
(3) capillary voltage: 2.8kV;
(4) desolventizing temperature degree: 500 DEG C;
(5) desolventizing airshed: 1000L/h;
(6) taper hole voltage is sampled: 65V;
(7) taper hole voltage is extracted: 4.0V;
(8) trap ions inducting device collision energy: 6.0V;
(9) trap ions inducting device flow: 1.5mL/min;
(10) mobility wave speed: 700m/sec;
(11) mobility wave height: 40V;
(12) mobility gas velocity: 90mL/min
(13) flight time mass spectrum mass analyzer quality acquisition range: m/z50to1500Da;
(14) flight time mass spectrum mass analyzer sweep time: 1.0sec;
(15) flight time mass spectrum mass analyzer sweep interval: 0.02sec;
(16) lock mass number reference corrected liquid: LEK solution, 200ng/mL, m/z556.2771Da.
Three, results and analysis
1, the UHV (ultra-high voltage) aqueous favoring interaction chromatographic resolution of ethoxylated dodecyl alcohol
This research adopts ACQUITYUPLCHSSHILIC chromatographic column (100mm × 2.1mm, 1.8 μm).As calculated, the alcohol water partition coefficient of ethoxylated dodecyl alcohol is between-7.03 (C 12eO 43) and 3.40 (C 12eO 5) between, display has very large hydrophobic difference.For realizing, from the short chain polymer had compared with strong-hydrophobicity to the multicomponent separation of the long chain polymer had compared with strongly hydrophilic, adopting gradient elution mode, carried out detailed optimization to condition of gradient elution.From Fig. 1 a, after experimental condition optimization, the order that the ethoxylated dodecyl alcohol of different polymerization degree increases progressively according to ethoxy number goes out peak successively, achieves good separation to each other, and its average divided degree is 1.94.Along with the attenuating of chromatographic column filler particle diameter, its separation efficiency improves very much, and when being 1.8 μm through comparing chromatographic column particle diameter, the degree of separation for ethoxylated dodecyl alcohol is respectively 1.53 times and 1.09 times of 3 μm and the 5 μm chromatographic columns of filling same nature filler.
2, the electron spray ionisation of ethoxylated dodecyl alcohol
Electron spray ionisation and Atmosphere Pressure Chemical Ionization (APCI) all have the research report being applied to ethoxylated dodecyl alcohol, and the application of usual electron spray ionisation is more.The present invention adopts direct injected mode, respectively under positive and negative two kinds of ionization mode, has investigated electron spray ionisation and the Atmosphere Pressure Chemical Ionization (APCI) ionization effect for ethoxylated dodecyl alcohol.Experimental result shows, under electron spray ionisation and Atmosphere Pressure Chemical Ionization (APCI) pattern, the ion distribution of ethoxylated dodecyl alcohol is totally similar, but the signal of electron spray ionisation is corresponding stronger.The acetonitrile-water mobile phase adopted in the hydrophilic interaction chromatography of UHV (ultra-high voltage) and electron spray ionisation can be compatible well.Found through experiments, in the electro-spray ionization process of ethoxylated dodecyl alcohol, can carry single electric charge, double charge and tricharged, the different electric charges of same degree of polymerization monomer band mass-to-charge ratio each other differs 44,22 and 14.7Da respectively simultaneously, this corresponding ethoxy group.
3, the ionic mobility of ethoxylated dodecyl alcohol is separated
First the separating effect of ethoxylated dodecyl alcohol under ionic mobility carrying different electric charge has been investigated by direct injected mode.Be optimized to obtain optimum separating effect to parameters such as mobility wave speed, mobility wave height, mobility airsheds respectively.Experimental result shows, even if in the chromatographic resolution situation do not had, still can realize ethoxylated dodecyl alcohol separation to a certain extent by means of only ionic mobility.The velocity of separation of ionic mobility is very fast, and the cycle completing a separating cycle only needs 6.64ms.By ionic mobility mass-spectrometric technique, effective separation of carrying different ethoxylated dodecyl alcohol ions can be realized.Fig. 2 a is the full scan mass spectrogram that ethoxylated dodecyl alcohol is separated without ionic mobility; Fig. 2 b, Fig. 2 c, Fig. 2 d are respectively the full scan mass spectrogram of single electric charge, double charge and the tricharged of ethoxylated dodecyl alcohol after ionic mobility separation, background correction.The half-peak breadth of carrying the difference polymerization ethoxylated dodecyl alcohol monomer spectrum peak of single electric charge, double charge and tricharged is respectively 0.21,0.17 and 0.11ms, and the average divided degree between monomer is respectively 0.56,0.39 and 0.35.Although in general, the degree of separation of ionic mobility can not compare favourably with traditional chromatographic resolution, and the quick separating of ionic mobility can cater between UHV (ultra-high voltage) aqueous favoring interaction chromatographic resolution time and flight time mass spectrum detection time well.
4, the full two dimensional separation analysis of the UHV (ultra-high voltage) of ethoxylated dodecyl alcohol hydrophilic interaction chromatography-ionic mobility mass spectrum
The ionic mobility mass spectrum that the hydrophilic interaction chromatography of UHV (ultra-high voltage) and second that first ties up is tieed up is carried out coupling, full two dimensional separation analysis is carried out to the ethoxylated dodecyl alcohol of different polymerization degree.Full two dimensional separation effect represents by three three-dimensional collection of illustrative plates that are mutually related, i.e. (Fig. 3 a), mass-to-charge ratio-UHV (ultra-high voltage) aqueous favoring interaction chromatographic retention figure (Fig. 3 b) and matter lotus be than – ionic mobility transit time figure (Fig. 3 c) for the ionic mobility transit time-UHV (ultra-high voltage) aqueous favoring interaction chromatographic retention figure of ethoxylated dodecyl alcohol.
From the ionic mobility transit time-UHV (ultra-high voltage) aqueous favoring interaction chromatographic retention figure of ethoxylated dodecyl alcohol, the hydrophilic interaction chromatography of UHV (ultra-high voltage) achieves the first dimension along transverse axis retention time direction according to the hydrophobic difference of ethoxylated dodecyl alcohol and is separated, and the difference of ionic mobility mass spectrum along longitudinal axis transit time direction according to ethoxylated dodecyl alcohol ionic mobility achieves two dimensional separation.The signal of the ethoxylated dodecyl alcohol component of different polymerization degree is confirmed with flight time mass spectrum.Having occurred three regions in Fig. 3 a, is the ethoxylated dodecyl alcohol of band single electric charge, double charge and tricharged respectively.Along with the increase of carrying electric charge number, the mobility of ion can increase, and collides pond by with the shorter time through ionic mobility.The ethoxylated dodecyl alcohol that the degree of polymerization is higher, molecular weight is larger, its structure relatively extends, and can occur more to collide with ionic mobility gas, therefore migration rate is slower; The degree of polymerization is lower, the ethoxylated dodecyl alcohol of molecular weight, and its structure is compacter, and collision cross section is long-pending less, and therefore migration rate is very fast.Can also find from Fig. 3 a, to carry an electric charge, the degree of polymerization of ethoxylated dodecyl alcohol at least will reach 13 more; To carry the 3rd electric charge, the degree of polymerization of ethoxylated dodecyl alcohol at least will reach 28.Infer that its reason may be for holding extra electric charge, polymkeric substance should be enough large with the increase of stable Coulomb force.
From the mass-to-charge ratio-UHV (ultra-high voltage) aqueous favoring interaction chromatographic retention figure of ethoxylated dodecyl alcohol, there is equidistant ion cluster of three rule distributions, the ethoxy group of the corresponding different number of every bit difference, mass-to-charge ratio 44,22 and 14.7 is differed respectively, i.e. an ethoxy between adjacent 2.The Zhi He of ethoxylated dodecyl alcohol also demonstrates in the first dimension is separated Bi – UHV (ultra-high voltage) aqueous favoring interaction chromatographic retention figure, and the ethoxylated dodecyl alcohol of different polymerization degree goes out peak successively according to hydrophobic order from high to low.
At the Zhi He of ethoxylated dodecyl alcohol in – ionic mobility transit time figure, single charge ion bunch, double-charge ion bunch and triply charged ion bunch (to each other with diagonal space) are there is, as can be seen here, entrained charge number, the ionic mobility for ethoxylated dodecyl alcohol is separated and plays a crucial role.For single electric charge and the multiple-charged ion of identical mass-to-charge ratio, the ionic mobility migration rate of multiple-charged ion is very fast.Be separated by ionic mobility, the desired separated of the ethoxylated dodecyl alcohol of different electric charge series can be realized, therefore, will simplification and the parsing of mass spectrogram be contributed to.
The orthogonality of 5, the hydrophilic interaction chromatography of UHV (ultra-high voltage)-ionic mobility mass spectrum full two dimensional separation analysis system and actual peak capacity evaluation study
Orthogonality and peak capacity are the important indicators evaluating full two dimensional separation system selectivity and separating power difference.Orthogonality is not only relevant with separation mechanism, also relevant with separation condition with the character of determinand.Related coefficient (r) is the conventional parameter for evaluating full two dimensional separation system orthogonality.When related coefficient is 1, represent first dimension be separated completely relevant with two dimensional separation, when related coefficient is 0, represent first dimension separation and two dimensional separation completely orthogonal, for the full two dimensional separation system of major part, its related coefficient is between 0 and 1.Peak dispersion angle (β) is that another evaluates the parameter of orthogonality, obtain by the arc cosine computing of related coefficient, when peak dispersion angle is 90 °, represent the first dimension separation and two dimensional separation completely orthogonal.For the full two dimensional separation system of UHV (ultra-high voltage) hydrophilic interaction chromatography-ionic mobility mass spectrum that this research institute builds, according to UHV (ultra-high voltage) aqueous favoring interaction chromatographic retention and the ionic mobility transit time of ethoxylated dodecyl alcohol, the related coefficient and the peak dispersion angle that calculate ethoxylated dodecyl alcohol are respectively 0.0224 and 88.72 °.
In theory, the peak capacity of the first dimension UHV (ultra-high voltage) aqueous favoring interaction chromatographic resolution is 195, the peak capacity that second dimension ionic mobility mass spectrum is separated is 40, and therefore, the theoretical peak capacity of the hydrophilic interaction chromatography of UHV (ultra-high voltage)-ionic mobility mass spectrum full two dimensional separation system is 7800.Average peak dispersion angle in view of this system is 88.72 °, calculating its actual peak capacity is 7713, individually use 40 times of the peak capacity of the first dimension UHV (ultra-high voltage) aqueous favoring interaction chromatographic resolution be used alone 193 times of the peak capacity that the second dimension ionic mobility mass spectrum is separated, peak capacity is greatly improved.
6, the calculating that ethoxylated dodecyl alcohol collision cross section is long-pending
This research selects polyalanine to be calibration substance, with its known collision cross section product value to ionic mobility transit time, draws single electric charge, double charge and tricharged three calibration curves respectively.And then, under identical experiment condition, ethoxylated dodecyl alcohol sample is tested, according to the calibrating curve equation released with polyalanine, extrapolate the collision cross section product value of ethoxylated dodecyl alcohol monomer of different electric charge, different polymerization degree, the results are shown in Table 2.Mass-to-charge ratio-ionic mobility transit time the figure of polyalanine is shown in Fig. 4, and the polyalanine calibration curve carrying single electric charge, double charge and tricharged is shown in Fig. 5.
Above-described embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various distortion that those of ordinary skill in the art make technical scheme of the present invention and improvement, all should fall in protection domain that claims of the present invention determines.

Claims (4)

1. the full two dimensional separation analytical approach of an ethoxylated dodecyl alcohol, it is characterized in that: the method adopting the hydrophilic interaction chromatography of UHV (ultra-high voltage) and ionic mobility mass spectrometry, construct the full two dimensional separation analysis system of ethoxylated dodecyl alcohol, achieve effective separation and the precise determination of complex target compound system, described method comprises the optimization of UHV (ultra-high voltage) aqueous favoring interaction chromatographic condition and ionic mobility Mass Spectrometry Conditions.
2. the full two dimensional separation analytical approach of ethoxylated dodecyl alcohol according to claim 1, is characterized in that: described UHV (ultra-high voltage) aqueous favoring interaction chromatographic condition is as follows:
(1) chromatographic column: WatersACQUITYUPLCHSSHILIC post, 100mm × 2.1mm, 1.8 μm;
(2) mobile phase: water-acetonihile gradient elution, gradient elution program is in table 1;
(3) flow velocity: 0.4mL/min;
(4) column temperature: 35 DEG C;
(5) sample chamber temperature: 10 DEG C;
(6) sample size: 10 μ L;
(7) pin liquid is washed: washing by force pin liquid is water, 200 μ L; Weak pin liquid of washing is acetonitrile, 600 μ L.
Table 1 gradient elution program
3. the full two dimensional separation analytical approach of ethoxylated dodecyl alcohol according to claim 1, is characterized in that: described ionic mobility Mass Spectrometry Conditions is as follows:
(1) ion gun: electron spray ionisation source;
(2) scan mode: positive ion mode;
(3) capillary voltage: 2.8kV;
(4) desolventizing temperature degree: 500 DEG C;
(5) desolventizing airshed: 1000L/h;
(6) taper hole voltage is sampled: 65V;
(7) taper hole voltage is extracted: 4.0V;
(8) trap ions inducting device collision energy: 6.0V;
(9) trap ions inducting device flow: 1.5mL/min;
(10) mobility wave speed: 700m/sec;
(11) mobility wave height: 40V;
(12) mobility gas velocity: 90mL/min;
(13) flight time mass spectrum mass analyzer quality acquisition range: m/z50to1500Da;
(14) flight time mass spectrum mass analyzer sweep time: 1.0sec;
(15) flight time mass spectrum mass analyzer sweep interval: 0.02sec;
(16) lock mass number reference corrected liquid: LEK solution, 200ng/mL, m/z556.2771Da.
4. the full two dimensional separation analytical approach of ethoxylated dodecyl alcohol according to claim 1, it is characterized in that: described method also comprises the long-pending computing method of ethoxylated dodecyl alcohol collision cross section, described computing method comprise the steps: to select polyalanine to be calibration substance, with the known collision cross section product value of described polyalanine to ionic mobility transit time, draw single electric charge, double charge and tricharged three calibration curves respectively; And then, under identical experiment condition, ethoxylated dodecyl alcohol is tested, according to the calibrating curve equation released with polyalanine, extrapolate the collision cross section product value of ethoxylated dodecyl alcohol monomer of different electric charge, different polymerization degree.
CN201510450876.0A 2015-07-28 2015-07-28 Laurinol polyoxyethylene ether fully two-dimensional separation analysis method Pending CN105067739A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106053588A (en) * 2016-06-02 2016-10-26 中国检验检疫科学研究院 Rapid detection method of alkylphenol ethoxylate on basis of ion mobility spectrometry
CN112362768A (en) * 2020-10-23 2021-02-12 北京民海生物科技有限公司 Method for measuring content of Berol 185 in sample by using liquid chromatography tandem mass spectrometry
CN115480016A (en) * 2022-10-12 2022-12-16 中国科学院兰州化学物理研究所 Liquid chromatography analysis and detection method of laurinol polyoxyethylene ether nonionic surfactant

Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106053588A (en) * 2016-06-02 2016-10-26 中国检验检疫科学研究院 Rapid detection method of alkylphenol ethoxylate on basis of ion mobility spectrometry
CN106053588B (en) * 2016-06-02 2018-08-17 中国检验检疫科学研究院 A kind of rapid detection method of the alkyl phenol polyoxyethylene ether based on ion mobility spectrometry
CN112362768A (en) * 2020-10-23 2021-02-12 北京民海生物科技有限公司 Method for measuring content of Berol 185 in sample by using liquid chromatography tandem mass spectrometry
CN112362768B (en) * 2020-10-23 2023-09-08 北京民海生物科技有限公司 Method for measuring Berol 185 content in sample by utilizing liquid chromatography-tandem mass spectrometry
CN115480016A (en) * 2022-10-12 2022-12-16 中国科学院兰州化学物理研究所 Liquid chromatography analysis and detection method of laurinol polyoxyethylene ether nonionic surfactant

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