CN102062766A - Method for measuring nonyl phenol in cosmetic - Google Patents
Method for measuring nonyl phenol in cosmetic Download PDFInfo
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- CN102062766A CN102062766A CN201010576977XA CN201010576977A CN102062766A CN 102062766 A CN102062766 A CN 102062766A CN 201010576977X A CN201010576977X A CN 201010576977XA CN 201010576977 A CN201010576977 A CN 201010576977A CN 102062766 A CN102062766 A CN 102062766A
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Abstract
The invention relates to a method for measuring nonyl phenol in cosmetic by liquid chromatography-mass spectrography/mass spectrography. The method is simple, convenient, quick, accurate and reliable, and detection limit, recovery rate and precision meet the requirements. The method is applied to the detection of a cosmetic sample, has high repeatability, and can be used for inspecting the nonyl phenol in the cosmetic.
Description
Technical field
The present invention relates to the assay method of nonyl phenol in a kind of cosmetics.
Background technology
Nonyl phenol:
English name: Nonylphenol
CAS：84852-15-3
Molecular formula: C
15H
24O
Molecular weight: 220.35
Structural formula:
Nonyl phenol is multiple mixture of isomers, and is colourless to faint yellow thick liquid, slightly phenol smell.Density 0.94～0.95g/cm
3(95%) 283～302 ℃ of boiling point.Water insoluble.Slightly be dissolved in sherwood oil.Be dissolved in acetone, phenixin, ethanol and chloroform.Be mainly used in and produce surfactant, also be used for fields such as antioxidant, textile auxiliary, oil dope, farm chemical emulgent, modifier, resin and rubber stabilizing agent.
Nonyl phenol is as typical phenols environmental estrogens, and it has caused people's extensive concern to the potential risk of environment and human health.Nonyl phenol is widely used as textile finshing agent, plastic plasticizer, industry and house detergent, agricultural chemicals and printing and dyeing emulsifying agent etc., and is used for synthetic non-ionics NPE in a large number.Nonyl phenol is as endocrine disruptor, and accumulation in vivo, and enter human body by food chain all can produce human cancer cell's growth and fecundity and to have a strong impact on, and is classified as preferential hazardous substance by European Union.Olso-Paris Convention (OSPAR) has also been listed nonyl phenol in priority pollutants matter register.
Summary of the invention
Technical matters solved by the invention provide a kind of accurately, reliable, the method for the micro-nonyl phenol in all higher cosmeticses of everyday use such as fast measuring cosmetics of detectability, the recovery and precision is beneficial to the quality monitoring of Related product.
For achieving the above object, the technical solution used in the present invention is as follows:
The assay method of nonyl phenol in a kind of cosmetics may further comprise the steps:
(1) sample is handled: take by weighing the about 0.5g of cosmetics sample, place 50mL tool plug conical flask, add mark storing solution in the 50 μ L, add 10mL methyl alcohol or absolute ethyl alcohol and methylene chloride mixed solution again, ultrasonic Extraction 30min in ultrasonic cleaner, extract is moved in the centrifuge tube, at the centrifugal 15min of 5000r/min speed, get supernatant 2mL after centrifugal, nitrogen slowly blows near to be done, with the dissolving of 30% methanol aqueous solution vortex, adopt the activation of 6mL methylene chloride and 6mL methyl alcohol, the isorrheic HLB Solid-Phase Extraction of 6mL column purification through in advance again; The 2mL sample solution uses 3mL 30% methanol aqueous solution to clean with sample on the 1mL/min flow velocity, and 6mL methanol dichloromethane mixed solution is wash-out at twice; The gained eluent slowly blows near with nitrogen to be done, and uses the 2mL methanol constant volume, measures for liquid chromatography-tandem mass spectrometry;
(2) measure: adopt liquid chromatography-mass spectrography/mass spectrometry method, wherein liquid phase chromatogram condition is: flow velocity: 0.25mL/min; Column temperature: 30 ℃; Sample size: 5 μ L; The mass spectrum condition is: capillary voltage: 1.5kV; Extraction voltage: 3V; Radio-frequency lens voltage: 0.5V; Ion source temperature: 150 ℃; Desolventizing temperature degree: 450 ℃;
(3) drawing standard working curve: accurately draw standard operation solution respectively and be mixed with the standard solution that concentration is 10 μ g/L, 50 μ g/L, 100 μ g/L, 250 μ g/L, 500 μ g/L, inner mark solution concentration is 50 μ g/L; Drawing respectively accurately 5 μ L and inject liquid chromatography-series connection quadrupole mass spectrometer, according to experimentizing under the above-mentioned analysis condition, is ordinate with the ratio of the peak area of quota ion, and the concentration corresponding with it is horizontal ordinate, the drawing standard working curve.
Method of the present invention, methyl alcohol or absolute ethyl alcohol described in the wherein said step (1) are preferably with the mixed volume ratio of methylene chloride mixed solution: methyl alcohol or absolute ethyl alcohol: methylene chloride=8: 2.
Liquid chromatography preferably adopts methyl alcohol-0.1% ammonia spirit as moving phase in the method for the present invention, wherein said step (2).
The inventive method adopts the nonyl phenol in liquid chromatography-mass spectrography/mass spectrometric determination cosmetics, and method is easy, quick, accurate, reliable, and detectability, the recovery and precision all meet the requirements.Method is applied to cosmetic sample and detects, and reappearance is good.Can, be used for the check of cosmetics nonyl phenol.
Embodiment
For further specifying the present invention, specify with the following Examples:
1, reagent and material
Except as otherwise noted, it is pure that agents useful for same is analysis, and water is secondary deionized water or double distilled water.
1.1 methyl alcohol: LC-MS level.
1.2 the nonyl phenol standard substance: purity is more than or equal to 98%.
1.34-n-the nonyl phenol standard substance: purity is more than or equal to 98%.
1.4 nonyl phenol standard inventory solution: accurately take by weighing an amount of nonyl phenol standard substance (being accurate to 0.1mg), being mixed with concentration with methyl alcohol is to put the standard inventory solution of 100mg/L.
1.54-n-mark stock solution in the nonyl phenol: accurately take by weighing an amount of 4-n-nonyl phenol standard substance (being accurate to 0.1mg), be mixed with the interior mark stock solution that concentration is 10mg/L with methyl alcohol.
2, instrument and equipment
2.1 liquid chromatography-series connection quadrupole mass spectrometer: be furnished with electric spray ion source.
2.2 ultrasound bath.
2.3 analytical balance: sensibility reciprocal is 0.001g and 0.001g.
2.4 hydro-extractor: greater than 5000r/min.
2.50.45 μ m organic system filtering membrane.
2.6 solid-phase extraction column (200mg, 6mL).
3, determination step
3.1 sample is handled
3.1.1 cream kind, loose powder, aqua class sample
Take by weighing the about 0.5g of cosmetics sample (being accurate to 0.001g), place 50mL tool plug conical flask, add mark storing solution in the 50 μ L, added 10mL methyl alcohol and methylene chloride mixed solution again (8: 2, V/V), ultrasonic Extraction 30min in ultrasonic cleaner, extract is moved in the centrifuge tube, at the centrifugal 15min of 5000r/min speed, get supernatant 2mL after centrifugal, nitrogen slowly blows near to be done, and dissolves with 30% methanol aqueous solution vortex again, adopt the activation of 6mL methylene chloride and 6mL methyl alcohol, the isorrheic HLB Solid-Phase Extraction of 6mL column purification through in advance.The 2mL sample solution is with sample on the 1mL/min flow velocity, uses 3mL 30% methanol aqueous solution to clean, and 6mL methanol dichloromethane mixed solution (8: 2, V/V) wash-out at twice.The gained eluent slowly blows near with nitrogen to be done, and uses the 2mL methanol constant volume, measures for liquid chromatography-tandem mass spectrometry.
3.1.2 lipstick class sample
Take by weighing the about 0.5g of cosmetics sample (being accurate to 0.001g), place 50mL tool plug conical flask, add mark storing solution in the 50 μ L, added 10mL absolute ethyl alcohol and methylene chloride mixed solution again (8: 2, V/V), ultrasonic Extraction 30min in ultrasonic cleaner, extract is moved in the centrifuge tube, at the centrifugal 15min of 5000r/min speed, get supernatant 2mL after centrifugal, nitrogen slowly blows near to be done, and dissolves with 30% methanol aqueous solution vortex again, adopt the activation of 6mL methylene chloride and 6mL methyl alcohol, the isorrheic HLB Solid-Phase Extraction of 6mL column purification through in advance.The 2mL sample solution is with sample on the 1mL/min flow velocity, uses 3mL 30% methanol aqueous solution to clean, and 6mL methanol dichloromethane mixed solution (8: 2, V/V) wash-out at twice.The gained eluent slowly blows near with nitrogen to be done, and uses the 2mL methanol constant volume, measures for liquid chromatography-tandem mass spectrometry.
3.2 measure
3.2.1 liquid chromatography-mass spectrography/mass spectrum condition
Because test result depends on employed instrument, therefore can not provide the general parameter of stratographic analysis.It is suitable adopting following operating conditions to be proved to be test.
(1) liquid phase chromatogram condition
A) chromatographic column: XBridge C
18Post, 150mm * 2.1mm (internal diameter), 3.5 μ m (particle diameter), or suitable person.
B) moving phase: methyl alcohol (A) and 0.1% ammonia spirit (B), gradient elution: 0～2.5min, 30%A～90%A; 2.5～3min, 90%A～95%A; 3～6min, 95%A; 6～8min, 95%A～30%A.
C) flow velocity: 0.25mL/min.
D) column temperature: 30 ℃.
E) sample size: 5 μ L.
(2) mass spectrum condition
A) ion gun: ESI.
B) ionization mode: negative ion mode.
C) capillary voltage: 1.5kV.
D) extraction voltage: 3V.
E) radio-frequency lens voltage: 0.5V.
F) ion source temperature: 150 ℃.
G) desolventizing temperature degree: 450 ℃.
H) data acquisition modes: multiple-reaction monitoring (MRM).
Table 1 mass spectrophotometry condition
3.2.2 the drafting of standard working curve
Accurately draw standard operation solution respectively and be mixed with the standard solution that concentration is 10 μ g/L, 50 μ g/L, 100 μ g/L, 250 μ g/L, 500 μ g/L, inner mark solution concentration is 50 μ g/L.Drawing respectively accurately 5 μ L and inject liquid chromatography-series connection quadrupole mass spectrometer, according to experimentizing under the above-mentioned analysis condition, is ordinate with the ratio of the peak area of quota ion, and the concentration corresponding with it is horizontal ordinate, the drawing standard working curve.
3.3 blank test
Except that not adding the sample, all undertaken by above-mentioned steps.
4, the result calculates
The result calculates by formula (1), and result of calculation keeps two-decimal:
In the formula:
W---the massfraction of nonyl phenol in the cosmetics, unit is every kilogram (mg/kg) of milligram;
C---the concentration of nonyl phenol from the sample solution that standard working curve is found, unit is every liter (mg/L) of milligram;
V---sample constant volume, unit is for rising (L);
The quality of m---sample, unit is gram (g).
5, the linear relationship of method and detection limit
5.1 linear relationship
Under the determined experiment condition of this method, get series of standards solution 10 μ g/L, 50 μ g/L, 100 μ g/L, 250 μ g/L, 500 μ g/L, ratio (Y-axis) with the peak area of nonyl phenol and internal standard compound is mapped to corresponding nonyl phenol concentration (X-axis), the result shows, nonyl phenol concentration is in 10 μ g/L～500 μ g/L scopes, the linear equation of nonyl phenol is Y=1.21X+1.76, and linearly dependent coefficient r=0.9996 is the good linear relation.When the nonyl phenol in the sample surpasses this range of linearity, can suitably strengthen the dilution of sample multiple.
5.2 the detection limit of method
Through the laboratory experiment to the method for inspection, the result shows that the mensuration lower bound (S/N=10) of method is 0.2mg/kg.
6, the recovery of method and precision
The experiment of this method recovery has been set three and has been added concentration by the interpolation situation in the common cosmetics, by the determined experiment condition of this method, each is added concentration carry out 6 experiments, and the nonyl phenol recovery is 83.1%～103.0%; Indoor precision experiment (n=6) records relative standard deviation 2.75%～9.24%.The results are summarized in table 2-5.
Table 2 cream kind sample recovery rate and precision experimental result
Table 3 aqua class sample recovery rate and precision experimental result
Table 4 loose powder class sample recovery rate and precision experimental result
Table 5 lipstick class sample recovery rate and precision experimental result
7, conclusion
Comprehensive above-mentioned situation, the recovery of this method of inspection, every technical indicators such as detectability and precision all meet the requirements, and method is applied to cosmetic sample and detects, and reappearance is good.The method of inspection that the present invention sets up is easy and simple to handle, the result is accurate, can be used for the check of nonyl phenol in the cosmetics.
Emphasis of the present invention is optimized above-mentioned experiment condition:
1, the selection of extracting method
1.1 extraction choice of Solvent
At dissimilar cosmetics, selecting cream kind, loose powder class, aqua class, lipstick class cosmetics is research object.The mixed solution of methyl alcohol, absolute ethyl alcohol and methylene chloride of having investigated methyl alcohol, absolute ethyl alcohol and different proportion respectively is as the extraction effect that extracts solution.The result shows, for cream kind, loose powder class, aqua class cosmetics, uses methyl alcohol and methylene chloride mixed solution (8: 2, volume fraction) as extraction effect the best of extracting solvent; For lipstick class cosmetics, use the extraction effect of absolute ethyl alcohol and methylene chloride mixed solution (8: 2, volume fraction) best.
1.2 the selection of extraction time
In order to obtain high as far as possible extraction efficiency and to reduce operation steps, adopt the ultrasonic Extraction mode that sample is extracted in the experiment.Investigated extraction time respectively and be the extraction effect under 15min, 20min, 25min, 30min, 35min, the 40min ultrasonic Extraction.The result shows that ultrasonic Extraction 30min can realize nonyl phenol is extracted fully.
2, the selection of Solid-Phase Extraction condition
According to bibliographical information, nonyl phenol is at C
18Show good reverse-phase chromatography retention behavior on the solid-phase extraction column, effect of extracting is better.In addition, Oasis HLB solid-phase extraction column is a kind of solid-phase extraction column based on the reverse-phase chromatography retention mechanism, and it has the C of ratio
18Adsorption capacity that solid-phase extraction column is higher and wideer advantages such as the pH scope of application.With Oasis HLB (6mL, 200mg) be solid-phase extraction column, investigated the eluting solvent of different mixing respectively: methyl alcohol, acetone-methyl alcohol mixed solution (1: 9, volume fraction), acetone-methyl alcohol mixed solution (3: 7, volume fraction), acetone-methyl alcohol mixed solution (5: 5, volume fraction), acetone-methyl alcohol-ethyl acetate mixture (4: 4: 2, volume fraction), acetone-methyl alcohol-ethyl acetate-formic acid (4: 4: 2: 0.1, volume fraction) the wash-out recovery, found that use acetone-methyl alcohol-ethyl acetate mixture (4: 4: 2, volume fraction) wash-out 6mL obtains the best recovery.
The Solid-Phase Extraction condition is as follows: adopt the activation of 6mL methylene chloride and 6mL methyl alcohol earlier, the 6mL water balance, the 2mL sample solution is with sample on the 1mL/min flow velocity, used 3mL methanol-water mixed solution (3: 7, volume fraction) cleans, acetone-methyl alcohol-ethyl acetate mixture (4: 4: 2, volume fraction) at twice, each 3mL wash-out.The gained eluent slowly dries up with nitrogen, uses the 2mL methanol constant volume, through filtering with microporous membrane, and feed flow phase chromatogram-series connection quadrupole rod mass spectroscopy.
3, the optimization of chromatographic condition
In liquid chromatography-mass spectrography was analyzed, moving phase was formed chromatographic peak profile and the degree of separation that not only influences target compound, also can influence its Ionization Efficiency and detection sensitivity.Experiment has been investigated the influence to the nonyl phenol degree of ionization of methanol-water and acetonitrile-water moving phase system in satisfied chromatographic resolution preferably.The result shows that the instrumental response value of methanol-water moving phase is higher than acetonitrile-water moving phase.Further comparative studies in methanol-water moving phase, add the influence of volatility additives such as 0.1% ammoniacal liquor, 5mmol/L ammonium formate, 5mmol/L ammonium acetate respectively.The result shows, has obtained optimum chromatographic resolution effect and mass signal response with methyl alcohol-0.1% ammonia spirit as moving phase.Because nonyl phenol has hydroxyl, can ionization go out a hydrogen ion in the solution at negative ion electrospray under pattern, when adding certain alkaline matter (as ammoniacal liquor) in the moving phase, will promote the ionization of target compound, thereby improve its Ionization Efficiency.Further investigated the influence of the ammoniacal liquor addition of different proportion, the addition of ammoniacal liquor changes to 0.5% result from 0.05% and shows that 0.1% ammoniacal liquor is optimum addition.
4, the optimization of mass spectrum condition
The chemi-ionization character that has phenolic hydroxyl group according to the phenols environmental estrogens, select for use ESI-as ionization mode, adopt flow injection pump continuous sample introduction mode to carry out the optimization of mass spectrum condition, experimental result shows, nonyl phenol can obtain [M-H] than high abundance under ion gun ESI-ionization mode
-Parent ion.Must reach 4 requirements of proving conclusively point according to the 2002/657/EC of European Union instruction regulation for the low liquid chromatography-mass spectrography conclusive evidence method of differentiating, adopt the daughter ion scan mode to carry out the second order ms analysis, daughter ion has been carried out optimized choice, determine quota ion and auxiliary qualitative ion, by optimizing capillary voltage, one-level taper hole voltage, secondary taper hole voltage, radio-frequency lens voltage, collision energy, mass spectrum parameters such as mass resolution, make the quasi-molecular ion of nonyl phenol and the ion pair intensity of feature fragmention generation reach maximum, high performance liquid chromatography and triple quadrupole bar mass spectrometer is online, to ion source temperature, temperature degree and flow desolvate, the taper hole airshed is optimized, and makes the Ionization Efficiency of test substance in the sample liquid reach best.
Above-described embodiment is described preferred implementation of the present invention; be not that scope of the present invention is limited; design under the prerequisite of spirit not breaking away from the present invention; various distortion and improvement that the common engineering technical personnel in this area make technical scheme of the present invention all should fall in the definite protection domain of claims of the present invention.
Claims (3)
1. the assay method of nonyl phenol in the cosmetics is characterized in that: may further comprise the steps:
(1) sample is handled: take by weighing the about 0.5g of cosmetics sample, place 50mL tool plug conical flask, add mark storing solution in the 50 μ L, add 10mL methyl alcohol or absolute ethyl alcohol and methylene chloride mixed solution again, ultrasonic Extraction 30min in ultrasonic cleaner, extract is moved in the centrifuge tube, at the centrifugal 15min of 5000r/min speed, get supernatant 2mL after centrifugal, nitrogen slowly blows near to be done, with the dissolving of 30% methanol aqueous solution vortex, adopt the activation of 6mL methylene chloride and 6mL methyl alcohol, the isorrheic HLB Solid-Phase Extraction of 6mL column purification through in advance again; The 2mL sample solution uses 3mL 30% methanol aqueous solution to clean with sample on the 1mL/min flow velocity, and 6mL methanol dichloromethane mixed solution is wash-out at twice; The gained eluent slowly blows near with nitrogen to be done, and uses the 2mL methanol constant volume, measures for liquid chromatography-tandem mass spectrometry;
(2) measure: adopt liquid chromatography-mass spectrography/mass spectrometry method, wherein liquid phase chromatogram condition is: flow velocity: 0.25mL/min; Column temperature: 30 ℃; Sample size: 5 μ L; The mass spectrum condition is: capillary voltage: 1.5kV; Extraction voltage: 3V; Radio-frequency lens voltage: 0.5V; Ion source temperature: 150 ℃; Desolventizing temperature degree: 450 ℃;
(3) drawing standard working curve: accurately draw standard operation solution respectively and be mixed with the standard solution that concentration is 10 μ g/L, 50 μ g/L, 100 μ g/L, 250 μ g/L, 500 μ g/L, inner mark solution concentration is 50 μ g/L; Drawing respectively accurately 5 μ L and inject liquid chromatography-series connection quadrupole mass spectrometer, according to experimentizing under the above-mentioned analysis condition, is ordinate with the ratio of the peak area of quota ion, and the concentration corresponding with it is horizontal ordinate, the drawing standard working curve.
2. assay method according to claim 1 is characterized in that: methyl alcohol or absolute ethyl alcohol described in the described step (1) with the mixed volume ratio of methylene chloride mixed solution are: methyl alcohol or absolute ethyl alcohol: methylene chloride=8: 2.
3. assay method according to claim 1 and 2 is characterized in that: liquid chromatography adopts methyl alcohol-0.1% ammonia spirit as moving phase in the described step (2).
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Cited By (5)
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| CN105301143A (en) * | 2015-11-30 | 2016-02-03 | 中国包装科研测试中心 | Method for detecting nonyl phenol in food packing material |
| CN106841448A (en) * | 2017-02-17 | 2017-06-13 | 孙丽 | A kind of detection method for polluting phenolic compound |
| CN111912930A (en) * | 2020-07-10 | 2020-11-10 | 甘肃省药品检验研究院 | Method for simultaneously determining 10 phthalic acid esters in aromatic cosmetics |
| WO2023274288A1 (en) * | 2021-06-29 | 2023-01-05 | 暨南大学 | Multi-component and high-throughput analysis method for plastic additives |
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| CN105223264A (en) * | 2015-09-21 | 2016-01-06 | 广东联捷生物科技有限公司 | Mark method, device and application in a kind of simulation of mass spectrum quantitative test |
| CN105301143A (en) * | 2015-11-30 | 2016-02-03 | 中国包装科研测试中心 | Method for detecting nonyl phenol in food packing material |
| CN106841448A (en) * | 2017-02-17 | 2017-06-13 | 孙丽 | A kind of detection method for polluting phenolic compound |
| CN111912930A (en) * | 2020-07-10 | 2020-11-10 | 甘肃省药品检验研究院 | Method for simultaneously determining 10 phthalic acid esters in aromatic cosmetics |
| WO2023274288A1 (en) * | 2021-06-29 | 2023-01-05 | 暨南大学 | Multi-component and high-throughput analysis method for plastic additives |
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