CN101975831B - 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
- Publication number
- CN101975831B CN101975831B CN201010560204A CN201010560204A CN101975831B CN 101975831 B CN101975831 B CN 101975831B CN 201010560204 A CN201010560204 A CN 201010560204A CN 201010560204 A CN201010560204 A CN 201010560204A CN 101975831 B CN101975831 B CN 101975831B
- Authority
- CN
- China
- Prior art keywords
- cosmetics
- liquid chromatography
- sample
- performance liquid
- concentration
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Images
Landscapes
- Cosmetics (AREA)
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, uses always and makes astringent, deodorant and the 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, filtrating 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: said A is 25mM sodium dihydrogen phosphate or the phosphate buffer solution that contains the 5mM TBAH, and pH 2.5; Said 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 said 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 said acetonitrile solution is 80%, also adds tetrahydrofuran before the said 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 said 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) appearance: be furnished with UV-detector or PDAD.
(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 gets part solution and is transferred in the 10mL tool plug plastic centrifuge tube, with the centrifugal 10min of 5000r/min; Supernatant supplies high-performance liquid chromatogram determination through 0.45 μ m filtering with microporous membrane.
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 to 15mL, ultrasonic Extraction 30min again; Get part solution and be transferred in the 10mL tool plug plastic centrifuge tube, with the centrifugal 15min of 5000r/min, supernatant supplies high-performance liquid chromatogram determination through 0.45 μ m filtering with microporous membrane.
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 supplies high-performance liquid chromatogram determination through 0.45 μ m filtering with microporous membrane.
(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 of using moving phase that zinc phenolsulfonate standard reserving solution stepwise dilution is obtained 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 appearance liquid that standard working curve is found, unit is every milliliter of microgram (μ g/mL);
V---the final constant volume of appearance liquid, unit are 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, and 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 describes 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 (9)
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, filtrating is carried out high-performance liquid chromatogram determination, and wherein: carrying out the used chromatographic column of high performance liquid chromatography is Kromasil C
18, 5 μ m, 250mm * 4.6mm internal diameter; The moving phase that high performance liquid chromatography detects is percent by volume 80%A and 20%B, and said A is 25mM sodium dihydrogen phosphate or the phosphate buffer solution that contains the 5mM TBAH, and pH 2.5, and said B is an acetonitrile.
2. method according to claim 1 is characterized in that: it is 230nm that said high performance liquid chromatography medium ultraviolet detects wavelength.
3. method according to claim 1 and 2 is characterized in that: said cosmetics are aqua, shampoo or cream frost, and the concentration of volume percent of said acetonitrile solution is 20%.
4. method according to claim 1 and 2 is characterized in that: said cosmetics are lipstick, and the concentration of volume percent of said acetonitrile solution is 80%, also add tetrahydrofuran before the said ultrasonic Extraction.
5. method according to claim 1 and 2 is characterized in that: said cosmetics are loose powder, and the concentration of volume percent of said acetonitrile solution is 80%.
6. method according to claim 1 is characterized in that: the said sample to be tested of 1g adds the 30mL acetonitrile solution.
7. method according to claim 4 is characterized in that: the said sample to be tested of 1g adds the 3mL tetrahydrofuran.
8. method according to claim 1 is characterized in that: said ultrasonic Extraction 30min.
9. method according to claim 1 is characterized in that: said centrifugal rotation speed is 5000r/min, centrifugation time 10min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010560204A CN101975831B (en) | 2010-11-25 | 2010-11-25 | Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201010560204A CN101975831B (en) | 2010-11-25 | 2010-11-25 | Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101975831A CN101975831A (en) | 2011-02-16 |
| CN101975831B true CN101975831B (en) | 2012-09-05 |
Family
ID=43575733
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201010560204A Expired - Fee Related CN101975831B (en) | 2010-11-25 | 2010-11-25 | Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101975831B (en) |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| AU2015260962B2 (en) * | 2014-05-13 | 2020-06-11 | Medimmune Limited | Anti-B7-H1 and anti-CTLA-4 antibodies for treating non-small cell lung cancer |
Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1638773A (en) * | 2001-07-30 | 2005-07-13 | 三菱制药株式会社 | Pharmaceutical preparations containing aminobenzene- sulfonic acid derivatives as the active ingredient |
| CN101169400A (en) * | 2006-10-24 | 2008-04-30 | 广东省保化检测中心有限公司 | High efficiency liquid chromatography detection method for sulpha drugs in cosmetic product |
| CN101169394A (en) * | 2007-02-09 | 2008-04-30 | 广东省保化检测中心有限公司 | Cosmetic product clindamycinum high efficiency liquid chromatography detection method |
| CN101169395A (en) * | 2007-05-10 | 2008-04-30 | 广东省保化检测中心有限公司 | Cosmetic product hydrocortisone high efficiency liquid chromatography detection method |
| CN101173912A (en) * | 2007-02-09 | 2008-05-07 | 广东省保化检测中心有限公司 | High efficiency liquid chromatography detecting method of erythromycin in cosmetic |
| CN101566603A (en) * | 2009-04-24 | 2009-10-28 | 刘江晖 | Method for detecting Cr(III) and Cr(5) in cosmetics by HPLC-ICP/MS combined technology |
| CN101625340A (en) * | 2009-06-25 | 2010-01-13 | 郑伟东 | High performance liquid chromatogram detecting method for detecting metaphenylene diamine in cosmetic oxidizing-type hair colorant |
| CN101644697A (en) * | 2009-06-10 | 2010-02-10 | 谱尼测试科技（北京）有限公司 | Detection method of IPBC in cosmetics |
| CN101718752A (en) * | 2009-11-10 | 2010-06-02 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method of residual polybrominated diphenyl ether in cosmetics with gas chromatography-mass spectrum method |
-
2010
- 2010-11-25 CN CN201010560204A patent/CN101975831B/en not_active Expired - Fee Related
Patent Citations (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1638773A (en) * | 2001-07-30 | 2005-07-13 | 三菱制药株式会社 | Pharmaceutical preparations containing aminobenzene- sulfonic acid derivatives as the active ingredient |
| CN101169400A (en) * | 2006-10-24 | 2008-04-30 | 广东省保化检测中心有限公司 | High efficiency liquid chromatography detection method for sulpha drugs in cosmetic product |
| CN101169394A (en) * | 2007-02-09 | 2008-04-30 | 广东省保化检测中心有限公司 | Cosmetic product clindamycinum high efficiency liquid chromatography detection method |
| CN101173912A (en) * | 2007-02-09 | 2008-05-07 | 广东省保化检测中心有限公司 | High efficiency liquid chromatography detecting method of erythromycin in cosmetic |
| CN101169395A (en) * | 2007-05-10 | 2008-04-30 | 广东省保化检测中心有限公司 | Cosmetic product hydrocortisone high efficiency liquid chromatography detection method |
| CN101566603A (en) * | 2009-04-24 | 2009-10-28 | 刘江晖 | Method for detecting Cr(III) and Cr(5) in cosmetics by HPLC-ICP/MS combined technology |
| CN101644697A (en) * | 2009-06-10 | 2010-02-10 | 谱尼测试科技（北京）有限公司 | Detection method of IPBC in cosmetics |
| CN101625340A (en) * | 2009-06-25 | 2010-01-13 | 郑伟东 | High performance liquid chromatogram detecting method for detecting metaphenylene diamine in cosmetic oxidizing-type hair colorant |
| CN101718752A (en) * | 2009-11-10 | 2010-06-02 | 浙江出入境检验检疫局检验检疫技术中心 | Detection method of residual polybrominated diphenyl ether in cosmetics with gas chromatography-mass spectrum method |
Non-Patent Citations (5)
| Title |
|---|
| 余年喜，等.HPLC 法检测抗青光眼新药(S)-OTS·HCl 水溶液的稳定性.《上海交通大学学报( 医学版)》.2010,第30卷(第7期),793-796. * |
| 王静,等.RP-HPLC 法测定羟苯磺酸钙分散片中的有关物质.《江苏药学与临床研究》.2006,第14卷(第6期),384-386. * |
| 程艳等.HPLC法测定化妆品中的烷基磺酸盐类表面活性剂.《2006（第九届）国际表面活性剂/洗涤剂会议》.2006,228-231. * |
| 郭栋,等.高效液相色谱法测定人血浆中轻苯磺酸钙的浓度.《药物分析杂志》.2008,第28卷(第8期),1252-1255. * |
| 马强.超高效液相色谱-串联质谱法同时测定.《分析化学》.2008,第36卷(第12期),1683-1689. * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN101975831A (en) | 2011-02-16 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102103128A (en) | Method for determining contents of formaldehyde, acetaldehyde and acetone in water-borne adhesives for cigarettes | |
| CN102539568A (en) | Ion chromatography method for detecting iodate and bromate in cosmetic | |
| CN103822976A (en) | Method for measuring 4-potassium methoxysalicylate in cosmetics | |
| CN100445726C (en) | Determining method of artemislnin content in artemisia apiacea | |
| CN103776939A (en) | Preparation detection method for substances related to rosuvastatin calcium preparation | |
| CN102955011A (en) | Gas chromatography detection method of ethylene glycol, diethylene glycol and menthol in toothpaste | |
| CN103954700A (en) | Method used for procyanidin content detection and identification | |
| CN101975831B (en) | Method for measuring zinc benzenesulfonate in cosmetics through high performance liquid chromatography (HPLC) | |
| CN104483406A (en) | High-efficiency liquid-phase chromatography detection method of L-arginine-alpha-ketoglutarate | |
| CN102955008B (en) | Method for detecting sulfonamide residue in eel by pressurized capillary electrochromatography | |
| CN103760278A (en) | High efficiency liquid chromatography method for simultaneously quantitatively detecting six flavonoid components in polygonum hydropiper | |
| CN103822977A (en) | Method for measuring seven functional components of liquorice in cosmetics | |
| CN101244240B (en) | Quantitative and qualitative analysis method for four turmeric soup preparations | |
| CN102818782B (en) | Determination method of total 2-(2-phenethyl) chromone compound content | |
| CN102305833A (en) | Measurement method of content of nitrites in polypropylene tow for cigarettes | |
| CN104090059A (en) | Method for simultaneously measuring eight components in edible flavors and fragrances | |
| CN107037152B (en) | The detection method of carminic acid content in a kind of gelatine capsule | |
| CN102507770A (en) | High performance liquid chromatography for detecting hexachlorophene in cosmetics | |
| CN103091437B (en) | Determination method of hesperidin content | |
| CN104568930A (en) | Method for determining content of catechuic acid in tea and tea products | |
| CN103235051A (en) | Method for determining colorant solvent green 7 in dry food packaging paper | |
| CN101169394A (en) | Cosmetic product clindamycinum high efficiency liquid chromatography detection method | |
| CN103424499B (en) | Method for detecting picrasma quassioides alkali content in picrasma quassioides | |
| Polati et al. | Preservatives in cosmetics. Analytical methods | |
| CN109342620A (en) | The method of means of derivation extraction Rapid Determination of Formaldehyde in Food |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20120905 Termination date: 20141125 |
|
| EXPY | Termination of patent right or utility model |