CN102680592A - Solution for measuring purity of para-phenylenediamine standard substance by using high performance liquid chromatograph and preparation method thereof - Google Patents
Solution for measuring purity of para-phenylenediamine standard substance by using high performance liquid chromatograph and preparation method thereof Download PDFInfo
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- CN102680592A CN102680592A CN201210106235XA CN201210106235A CN102680592A CN 102680592 A CN102680592 A CN 102680592A CN 201210106235X A CN201210106235X A CN 201210106235XA CN 201210106235 A CN201210106235 A CN 201210106235A CN 102680592 A CN102680592 A CN 102680592A
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Abstract
The invention relates to a solution for measuring purity of a para-phenylenediamine standard substance by using a high performance liquid chromatograph and a preparation method thereof. The solution for measuring the purity of the para-phenylenediamine standard substance by using the high performance liquid chromatograph consists of chromatography pure methanol, sodium sulfite with concentration of 1-10 mug/mL, and para-phenylenediamine standard substance with concentration of 500-2000 mug/mL. The preparation method of the solution for measuring the purity of the para-phenylenediamine standard substance by using the high performance liquid chromatograph comprises the steps of at the temperature of 4-10 DEG C, adding sodium sulfite and para-phenylenediamine standard substance in sequence to chromatography pure methanol. The method provided by the invention can accurately and stably measure the purity of the para-phenylenediamine standard substance, ensure the impurities in para-phenylenediamine standard substance to be detected by the high performance liquid chromatograph, and effectively guarantee the quantity transmission and the safety and sanitation quality of the detecting work for the poisonous and harmful chemicals in daily life.
Description
Technical field
The present invention relates to metrology and measurement standard transmission of quantity value technical field, especially relate to a kind of high performance liquid chromatograph and measure solution of p-phenylenediamine (PPD) standard substance purity and preparation method thereof.
Background technology
Along with people's growth in the living standard, cosmetics become people's daily life must the indispensable consumer goods.Begin from nineteen ninety; The cosmetics consumption market of China has been marched toward the period of a Rapid Expansion especially; According to statistics; Cosmetics consumption average year in recent years increases progressively 12.9%, and the spending share that a feast for the eyes cosmetics are consumed in people's daily life kind remains high, and China becomes the competitive market that each big well-known cosmetics company of the world can not lack gradually.Yet people have also run into many puzzlements when pursuing U.S.A.All kinds of chemical addition agent materials that use or excess are used in the cosmetics in recent years cause the report of various acute or chronic hazard of common occurrence to health, as use some heavy metal elements meetings carcinogenic; Use some hormone can cause human body skin and human body hormone to change; The use of part antibiotic can destroy the normal flora of skin surface; Excessive use antiseptic, sun-screening agent can produce the effect of running counter to desire to human body.
In order to ensure the people's quality of life, the government department of countries in the world has formulated more and more stricter instruction in succession and has controlled and variously in the cosmetics can bring the adjuvant of harm to health.The important means of effective healthy cosmetics of everyday use safety and sanitation quality is the content of the relevant poisonous and harmful chemicals of monitoring, and the current relevant criterion material that generally uses carries out the work of transmission of quantity value, with accuracy, the consistance that realizes measuring.
P-phenylenediamine (PPD) (p-Phenylenediamine) is the white plates crystallization, in air, is oxidized to aubergine or dark brown very soon.This material has very strong sensitization, can cause contact dermatitis, eczema, bronchial astehma, and carcinogenesis is arranged.P-phenylenediamine (PPD) is a kind of the most frequently used colorant in the cosmetics of everyday use such as hair dyeing, and is because its harm to human body, disabled in the last few years or limit the use of.Mensuration as the standard substance purity of one of the bottleneck of daily chemical products safe and sanitary technology; When comprising with high performance liquid chromatograph mensuration p-phenylenediamine (PPD) standard substance purity, solution of p-phenylenediamine (PPD) standard substance purity and preparation method thereof is standard substance purity testing result key factor accurately.
When prior art adopts high performance liquid chromatograph to measure p-phenylenediamine (PPD) standard substance purity, be directly in chromatographically pure methyl alcohol, to add the p-phenylenediamine (PPD) standard substance to be prepared into solution, carry out high performance liquid chromatography and detect.Because p-phenylenediamine (PPD) is easy to by airborne dioxygen oxidation; When not adding sodium sulphite; And when not controlling temperature, the chromatogram that high performance liquid chromatograph detects is easy to occur the oxidized peak of p-phenylenediamine (PPD), As time goes on; Oxidized peak is more and more stronger, and the peak of p-phenylenediamine (PPD) standard substance is more and more littler.And solution meeting change color in 30min, thereby cause high-performance liquid chromatogram determination p-phenylenediamine (PPD) standard substance purity result inaccurate.
Summary of the invention
Technical matters to be solved by this invention provide a kind ofly can stablize more, truly, accurate high performance liquid chromatograph measures solution of p-phenylenediamine (PPD) standard substance purity and preparation method thereof.The present invention solves the technical scheme that its technical matters adopts: a kind of high performance liquid chromatograph is measured the solution of p-phenylenediamine (PPD) standard substance purity, and it is that the sodium sulphite of 1-10 μ g/mL and p-phenylenediamine (PPD) standard substance that concentration is 500-2000 μ g/mL are formed by chromatographically pure methyl alcohol, concentration.Under 4-10 ℃ temperature, in chromatographically pure methyl alcohol, add sodium sulphite and p-phenylenediamine (PPD) standard substance successively.Technical matters to be solved by this invention also can further be solved through following technical scheme: the concentration of sodium sulphite is 1 μ g/mL, 3 μ g/mL, 5 μ g/mL, 8 μ g/mL or 10 μ g/mL; The concentration of p-phenylenediamine (PPD) standard substance is 500 μ g/mL, 800 μ g/mL, 1000 μ g/mL, 1500 μ g/mL or 2000 μ g/mL; Temperature is 4 ℃, 6 ℃, 8 ℃ or 10 ℃.Chromatographically pure methyl alcohol among the present invention is dilution, is used to dilute sodium sulphite and p-phenylenediamine (PPD) standard substance, and it is oxidized in air that sodium sulphite can slow down the p-phenylenediamine (PPD) standard substance, and the p-phenylenediamine (PPD) standard substance is used to measure the magnitude tracing transmission.Chromatographically pure methyl alcohol of the present invention, sodium sulphite and p-phenylenediamine (PPD) standard substance all can be buied in Chinese home market.The present invention is owing to adopt technique scheme; Slowed down the speed of p-phenylenediamine (PPD) oxidation by air; And the concentration that makes the p-phenylenediamine (PPD) standard substance is 500-2000 μ g/mL; Make high performance liquid chromatograph can be accurately, the purity of stable measuring p-phenylenediamine (PPD) standard substance, guaranteed that the impurity in the p-phenylenediamine (PPD) standard substance all can be detected by high performance liquid chromatograph, and be no more than the range ability that high performance liquid chromatograph detects; The transmission of quantity value and the safety and sanitation quality of the poisonous and harmful chemicals testing in the cosmetics of everyday use have been ensured effectively; Prevent the trade dispute that exceeds standard and cause because of related substances, promoted China's standard substance development and the advantage in cosmetics of everyday use trade monitoring, safeguarded the economic interests of China.
Description of drawings
Below in conjunction with accompanying drawing and specific embodiment of the present invention the present invention is described in further detail:
Fig. 1 is the chromatogram of prior art.
Fig. 2, Fig. 3, Fig. 4 are respectively the chromatograms of the embodiment of the invention 2, embodiment 8, embodiment 10.
Embodiment
| ? | Embodiment 1 | |
Embodiment 3 | |
Embodiment 5 |
| Chromatographically |
100 |
100 |
100 |
100 |
100 mL |
| Sodium sulphite | 100μg | 800μg | 500μg | 300μg | 1000μg |
| The p-phenylenediamine (PPD) standard substance | 200000μg | 80000μg | 100000μg | 150000μg | 50000μg |
| ? | |
Embodiment 7 | |
Embodiment 9 | |
| Chromatographically |
100 |
100 |
100 |
100 |
100 mL |
| Sodium sulphite | 100μg | 800μg | 500μg | 300μg | 1000μg |
| The p-phenylenediamine (PPD) standard substance | 50000μg | 150000μg | 80000μg | 100000μg | 200000μg |
Embodiment 11: under 4 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 100 μ g and the p-phenylenediamine (PPD) standard substance of 200000 μ g successively.
Embodiment 12: under 6 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 800 μ g and the p-phenylenediamine (PPD) standard substance of 8000 μ g successively.
Embodiment 13: under 8 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 500 μ g and the p-phenylenediamine (PPD) standard substance of 100000 μ g successively.
Embodiment 14: under 10 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 300 μ g and the p-phenylenediamine (PPD) standard substance of 150000 μ g successively.
Embodiment 15: under 10 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 1000 μ g and the p-phenylenediamine (PPD) standard substance of 50000 μ g successively.
Embodiment 16: under 4 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 100 μ g and the p-phenylenediamine (PPD) standard substance of 50000 μ g successively.
Embodiment 17: under 6 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 800 μ g and the p-phenylenediamine (PPD) standard substance of 150000 μ g successively.
Embodiment 18: under 8 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 500 μ g and the p-phenylenediamine (PPD) standard substance of 80000 μ g successively.
Embodiment 19: under 10 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 300 μ g and the p-phenylenediamine (PPD) standard substance of 100000 μ g successively.
Embodiment 20: under 10 ℃ temperature, in the chromatographically pure methyl alcohol of 100 mL, add the sodium sulphite of 1000 μ g and the p-phenylenediamine (PPD) standard substance of 200000 μ g successively.
The said goods embodiment 1-10 corresponds respectively to method embodiment 11-20.
Claims (5)
1. a high performance liquid chromatograph is measured the solution of p-phenylenediamine (PPD) standard substance purity, it is characterized in that: it is that the sodium sulphite of 1-10 μ g/mL and p-phenylenediamine (PPD) standard substance that concentration is 500-2000 μ g/mL are formed by chromatographically pure methyl alcohol, concentration.
2. a kind of high performance liquid chromatograph according to claim 1 is measured the solution of p-phenylenediamine (PPD) standard substance purity, and it is characterized in that: the concentration of sodium sulphite is 1 μ g/mL, 3 μ g/mL, 5 μ g/mL, 8 μ g/mL or 10 μ g/mL.
3. a kind of high performance liquid chromatograph according to claim 1 is measured the solution of p-phenylenediamine (PPD) standard substance purity, and it is characterized in that: the concentration of p-phenylenediamine (PPD) standard substance is 500 μ g/mL, 800 μ g/mL, 1000 μ g/mL, 1500 μ g/mL or 2000 μ g/mL.
4. the solution manufacturing method of a high performance liquid chromatograph mensuration p-phenylenediamine (PPD) standard substance purity as claimed in claim 1 is characterized in that: under 4-10 ℃ temperature, in chromatographically pure methyl alcohol, add sodium sulphite and p-phenylenediamine (PPD) standard substance successively.
5. a kind of solution manufacturing method according to claim 4 is characterized in that: temperature is 4 ℃, 6 ℃, 8 ℃ or 10 ℃.
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| CN201210106235XA CN102680592A (en) | 2012-06-08 | 2012-06-08 | Solution for measuring purity of para-phenylenediamine standard substance by using high performance liquid chromatograph and preparation method thereof |
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| CN201210106235XA CN102680592A (en) | 2012-06-08 | 2012-06-08 | Solution for measuring purity of para-phenylenediamine standard substance by using high performance liquid chromatograph and preparation method thereof |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104777245A (en) * | 2015-03-13 | 2015-07-15 | 淮安市匹克斯生物科技有限公司 | Cosmetic oxidative hair dye detection method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060075580A1 (en) * | 2004-10-12 | 2006-04-13 | Unilever Home & Personal Care Usa, Division Of Conopco, Inc. | Two step hair coloring compositions delivering deeper, long-lasting color |
| CN101545891A (en) * | 2009-04-24 | 2009-09-30 | 中华人民共和国苏州出入境检验检疫局 | Method for concurrent measurement of p-phenylenediamine, o-phenylenediamine, hydroquinone and resorcinol in oxygenize type hair dyes agent |
-
2012
- 2012-06-08 CN CN201210106235XA patent/CN102680592A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20060075580A1 (en) * | 2004-10-12 | 2006-04-13 | Unilever Home & Personal Care Usa, Division Of Conopco, Inc. | Two step hair coloring compositions delivering deeper, long-lasting color |
| CN101545891A (en) * | 2009-04-24 | 2009-09-30 | 中华人民共和国苏州出入境检验检疫局 | Method for concurrent measurement of p-phenylenediamine, o-phenylenediamine, hydroquinone and resorcinol in oxygenize type hair dyes agent |
Non-Patent Citations (2)
| Title |
|---|
| 张辉 等: "染发类化妆品中10种苯二胺类化合物的气相色谱法测定", 《香料香精化妆品》 * |
| 肖怀 等: "天然染发剂中对苯二胺定量分析", 《大理学院学报》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104777245A (en) * | 2015-03-13 | 2015-07-15 | 淮安市匹克斯生物科技有限公司 | Cosmetic oxidative hair dye detection method |
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Application publication date: 20120919 |