CN101975831A - Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) - Google Patents
Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) Download PDFInfo
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- CN101975831A CN101975831A CN 201010560204 CN201010560204A CN101975831A CN 101975831 A CN101975831 A CN 101975831A CN 201010560204 CN201010560204 CN 201010560204 CN 201010560204 A CN201010560204 A CN 201010560204A CN 101975831 A CN101975831 A CN 101975831A
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Abstract
The invention discloses a method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC), comprising the following steps of: adding an acetonitrile aqueous solution into a sample to be tested, ultrasonically extracting, centrifuging an extraction solution, filtering supernate with a millipore filter, and measuring the filtrate with the HPLC. The method for measuring the zinc benzenesulfonate in cosmetics through the HPLC is rapid and has low detection limit and high recovery rate.
Description
Technical field
The present invention relates to the method for zinc phenolsulfonate in a kind of high effective liquid chromatography for measuring cosmetics.
Background technology
Zinc phenolsulfonate is generally white or light yellow crystalline powder, and is soluble in water, is dissolved in organic reagents such as methyl alcohol, ethanol and acetonitrile, is exposed to become pink in the air.Zinc phenolsulfonate can stimulate eyes and skin, and sucking zinc phenolsulfonate dust can stimulate nose and throat, and heavy dose of the absorption has the vomiting effect.Zinc phenolsulfonate has good convergence and restraining and sterilizing bacteria effect, is commonly used for astringent, deodorant and antiperspirant in the cosmetics.According to the regulation of China's " hygienic standards for cosmetics ", " cosmetics health standard ", zinc phenolsulfonate is that component limits the use of material in the cosmetics.
Less to the research report of zinc phenolsulfonate in the cosmetics both at home and abroad at present.European Union once had report to utilize the content of 4-hydroxy benzene sulfonic acid in the iodometric determination cosmetics, thereby indirect calculation goes out the content of zinc phenolsulfonate and zinc in the cosmetics.The operation of this method is comparatively loaded down with trivial details, and with 4-hydroxyl phenol sulfonic acid be standard can not the complete reaction cosmetic base in the content of zinc phenolsulfonate, have certain deviation.
Summary of the invention
The purpose of this invention is to provide that a kind of detectability is low, the recovery is high, the method for zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics fast.
The method of zinc phenolsulfonate comprises the steps: in the high effective liquid chromatography for measuring cosmetics provided by the present invention
In sample to be tested, add acetonitrile solution, ultrasonic Extraction, extract is centrifugal, the supernatant filtering with microporous membrane, filtrate is carried out high-performance liquid chromatogram determination.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, wherein the moving phase of high performance liquid chromatography detection is percent by volume 80%A and 20%B: described A is 25mM sodium dihydrogen phosphate or the phosphate buffer solution that contains the 5mM TBAH, and pH 2.5; Described B is an acetonitrile.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, it is 230nm that wherein said high performance liquid chromatography medium ultraviolet detects wavelength.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, wherein said cosmetics are aqua, shampoo or cream frost, and the concentration of volume percent of described acetonitrile solution is 20%.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, wherein said cosmetics are lipstick, the concentration of volume percent of described acetonitrile solution is 80%, also adds tetrahydrofuran before the described ultrasonic Extraction.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, wherein said cosmetics are loose powder, the concentration of volume percent of described acetonitrile solution is 80%.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, wherein said 1g sample to be tested adds the 30mL acetonitrile solution.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, wherein said 1g sample to be tested adds the 3mL tetrahydrofuran.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, wherein said ultrasonic Extraction 30min.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, wherein said centrifugal rotation speed is 5000r/min, centrifugation time 10min.
The method of zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics of the present invention, detecting of zinc phenolsulfonate is limited to 24mg/kg in aqua and the shampoo sample, detecting of zinc phenolsulfonate is limited to 120mg/kg in cream frost and the lipstick sample, detecting of zinc phenolsulfonate is limited to 60mg/kg in the loose powder sample, the recovery between 93.63%～99.09%, relative standard deviation 0.57～3.87%.
Description of drawings
Fig. 1 is for adding the aqua sample chromatogram figure of detection limit concentration.
Fig. 2 is an aqua blank sample chromatogram.
Fig. 3 is for adding the shampoo sample chromatogram figure of detection limit concentration.
Fig. 4 is a shampoo blank sample chromatogram.
Fig. 5 is for adding the cream frost sample chromatogram figure of detection limit concentration.
Fig. 6 is a cream frost blank sample chromatogram.
Fig. 7 is for adding the lipstick sample chromatogram figure of detection limit concentration.
Fig. 8 is a lipstick blank sample chromatogram.
Fig. 9 is for adding the loose powder sample chromatogram figure of detection limit concentration.
Figure 10 is a loose powder blank sample chromatogram.
Embodiment
Zinc phenolsulfonate standard items: eight water zinc phenolsulfonate crystalline powders.
Zinc phenolsulfonate standard reserving solution: accurately take by weighing zinc phenolsulfonate standard substance 100mg, place the brown volumetric flask of 100mL, with dissolve with methanol and be settled to scale, shake up, be mixed with the standard reserving solution that concentration is respectively 1000 μ g/mL, keep in Dark Place in 4 ℃.
High performance liquid chromatography (HPLC) instrument: be furnished with UV-detector or diode array detector.
(1) sample preparation
Aqua, shampoo, cream kind sample: take by weighing 0.5g (being accurate to 0.001g) sample in 50mL tool plug conical flask, add 15mL 20% acetonitrile solution, ultrasonic Extraction 30min, getting part solution is transferred in the 10mL tool plug plastic centrifuge tube, with the centrifugal 10min of 5000r/min, supernatant is through 0.45 μ m filtering with microporous membrane, for high-performance liquid chromatogram determination.
Lipstick class sample: take by weighing 0.5g (being accurate to 0.001g) sample in 50mL tool plug conical flask, add the 1.5mL tetrahydrofuran, ultrasonic Extraction 10min adds 80% acetonitrile solution again to 15mL, ultrasonic Extraction 30min; Get part solution and be transferred in the 10mL tool plug plastic centrifuge tube, with the centrifugal 15min of 5000r/min, supernatant is through 0.45 μ m filtering with microporous membrane, for high-performance liquid chromatogram determination.
Loose powder class sample: take by weighing 0.5g (being accurate to 0.001g) sample in 50mL tool plug conical flask, add 15mL 80% acetonitrile solution, ultrasonic Extraction 30min; Get part solution and be transferred in the 10mL tool plug plastic centrifuge tube, with the centrifugal 10min of 5000r/min, supernatant is through 0.45 μ m filtering with microporous membrane, for high-performance liquid chromatogram determination.
(2) condition determination
A) chromatographic column: Kromasil C
18, 5 μ m, 250mm * 4.6mm (i.d.).
B) moving phase
80%A:5mM TBAH+25mM sodium dihydrogen phosphate/phosphate buffer solution, pH 2.5
20%B: acetonitrile
C) flow velocity: 1.0mL/min.
D) column temperature: 30 ℃.
E) wavelength: 230nm.
F) sample size: 10 μ L.
(3) drafting of typical curve
The concentration that zinc phenolsulfonate standard reserving solution stepwise dilution is obtained with moving phase is the standard operation liquid of 0.5,1,2,5,10,20,50 μ g/mL, and concentration is sample detection from low to high, with peak area-concentration mapping, obtains the typical curve regression equation.
The phenolsulfonic acid zinc concentration is in 0.5～50 μ g/mL scope, and the concentration peak area value corresponding with it is the good linear relation, and related coefficient is 0.9998.
The gained linear equation is y=24.9510x+27.7741
(4) calculate
The result is calculated as follows:
In the formula:
The percentage composition of zinc phenolsulfonate (massfraction) in W-sample;
C---phenolsulfonic acid zinc concentration from the sample liquid that standard working curve is found, unit is every milliliter of microgram (μ g/mL);
V---the final constant volume of sample liquid, unit is milliliter (mL);
The quality of m---sample, unit is gram (g).
Detect in aqua and the shampoo sample and be limited to 24mg/kg, quantitatively be limited to 30mg/kg; Detect in cream frost and the lipstick sample and be limited to 120mg/kg, quantitatively be limited to 140mg/kg; Detect in the loose powder sample and be limited to 60mg/kg, quantitatively be limited to 90mg/kg.
(5) recovery and precision
By the interpolation situation in the common cosmetics; set three and added concentration; each is added concentration carry out 6 tests; Fig. 2,4,6,8,10 is five kinds of cosmetics blank sample chromatograms; Fig. 1,3,5,7,9 looks for spectrogram for blank sample adds the detection limit concentration standard, and the recovery and degree of accuracy result are in table 1.
Table 1. phenolsulfonic acid zinc recovery and Precision test result
Above 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 (10)
1. the method for zinc phenolsulfonate in the high effective liquid chromatography for measuring cosmetics comprises the steps:
In sample to be tested, add acetonitrile solution, ultrasonic Extraction, extract is centrifugal, the supernatant filtering with microporous membrane, filtrate is carried out high-performance liquid chromatogram determination.
2. method according to claim 1 is characterized in that: the moving phase that high performance liquid chromatography detects is percent by volume 80%A and 20%B: described A is 25mM sodium dihydrogen phosphate or the phosphate buffer solution that contains the 5mM TBAH, and pH 2.5; Described B is an acetonitrile.
3. method according to claim 1 is characterized in that: it is 230nm that described high performance liquid chromatography medium ultraviolet detects wavelength.
4. according to arbitrary described method in the claim 1 to 3, it is characterized in that: described cosmetics are aqua, shampoo or cream frost, and the concentration of volume percent of described acetonitrile solution is 20%.
5. according to arbitrary described method in the claim 1 to 3, it is characterized in that: described cosmetics are lipstick, and the concentration of volume percent of described acetonitrile solution is 80%, also add tetrahydrofuran before the described ultrasonic Extraction.
6. according to arbitrary described method in the claim 1 to 3, it is characterized in that: described cosmetics are loose powder, and the concentration of volume percent of described acetonitrile solution is 80%.
7. method according to claim 1 is characterized in that: the described sample to be tested of 1g adds the 30mL acetonitrile solution.
8. method according to claim 5 is characterized in that: the described sample to be tested of 1g adds the 3mL tetrahydrofuran.
9. method according to claim 1 is characterized in that: described ultrasonic Extraction 30min.
10. method according to claim 1 is characterized in that: described centrifugal rotation speed is 5000r/min, centrifugation time 10min.
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| CN103149304A (en) * | 2012-12-01 | 2013-06-12 | 云南白药集团股份有限公司 | Method for accurately detecting flavonoid content in pollen |
| TWI707692B (en) * | 2014-05-13 | 2020-10-21 | 英商梅迪繆思有限公司 | Anti-b7-h1 and anti-ctla-4 antibodies for treating non-small cell lung cancer |
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| CN103149304B (en) * | 2012-12-01 | 2016-01-20 | 云南白药集团股份有限公司 | The method of the flavones content in a kind of accurate detection pollen |
| TWI707692B (en) * | 2014-05-13 | 2020-10-21 | 英商梅迪繆思有限公司 | Anti-b7-h1 and anti-ctla-4 antibodies for treating non-small cell lung cancer |
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