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 PDF

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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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standard substance
ni
amine
purity
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CN201210106235XA
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吴建军
李�杰
王虎
田玉平
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上海市计量测试技术研究院
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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

一种高效液相色谱仪测定对苯ニ胺标准物质纯度的溶液及其制备方法 One kind of high performance liquid chromatography assay solution and a preparation method of the amine standard substance benzene purity Ni

技术领域 FIELD

[0001] 本发明涉及计量测试标准量值传递技术领域,尤其是涉及ー种高效液相色谱仪测定对苯ニ胺标准物质纯度的溶液及其制备方法。 [0001] The present invention relates to measuring and testing standard value transfer technologies, and particularly relates to apparatus ー species Determination standard substance solution of the amine purity terephthalic Ni and preparation method.

背景技术 Background technique

[0002] 随着人们生活水平的提高,化妆品成为人们日常生活必不可缺少的消费品。 [0002] With the improvement of people's living standards, cosmetics become an everyday consumer goods indispensable. 自1990年开始,中国的化妆品消费市场更是迈入了ー个快速扩张的时期,据统计,近几年的化妆品消费平均年递增12. 9%,琳琅满目的化妆品消费在人们日常生活种的开支份额居高不下,中国逐渐成为世界各大知名化妆品公司不可缺失的竞争市场。 Since 1990, China's cosmetics consumer market is entering a period of rapid expansion ー months, according to statistics, the consumption of cosmetics in recent years the average annual increase of 12.9 percent, daily life kind of consumer spending in an array of cosmetics share remains high, China has become the world's leading cosmetics company can not be missing competitive market. 然而,人们在追求美的同吋,也遇到了不少困扰。 However, people in the pursuit of beauty with inches, also encountered a lot of problems. 近年来化妆品中使用或超量使用的各类化学添加剂物质对人体健康造成多种急性或慢性危害的报道屡见不鲜,如使用ー些重金属元素会致癌;使用某些激素可造成人体皮肤和肌体激素变化;部分抗菌素的使用会破坏皮肤表面的正常菌群;过量使用防腐剤、防晒剂会对人体产生适得其反的作用。 In recent years, the use of cosmetics or excessive use of various types of chemical additives substances cause a variety of acute or chronic harm to human health coverage are common, such as the use ー some heavy metals cause cancer; the use of certain hormones can cause skin and hormonal changes in the body ; use of antibiotics will destroy part of the normal flora of the skin surface; excess corrosion Ji, sunscreen would be counterproductive in the human body.

[0003] 为了保障人民的生活质量,世界各国的政府部门相继制定了越来越严格的指令来控制化妆品中各种能给人体健康带来危害的添加剤。 [0003] In order to protect the quality of life of the people, governments around the world have developed increasingly strict instructions to control a variety of cosmetics to give harm to human health be added Ji. 有效的健康日化用品安全卫生质量的重要手段是监控相关有毒有害化学品的含量,当前普遍使用相关标准物质来进行量值传递的工作,以实现测量的准确性、一致性。 Effective health of supplies important means of health and safety is to monitor the quality of content related to toxic and hazardous chemicals, the current widespread use of relevant reference materials to carry out work of value transfer, to achieve measurement accuracy, consistency.

[0004] 对苯ニ胺(p-Pheny Ienediamine )为白色片状结晶,在空气中很快被氧化成紫红色或深褐色。 [0004] p ni amine (p-Pheny Ienediamine) as a white flaky crystals in the air is rapidly oxidized to brown or dark purple. 该物质具有很强的致敏作用,可引起接触性皮炎、湿疹、支气管哮喘,且有致癌作用。 This material has a strong sensitization, can cause contact dermatitis, eczema, asthma, and have carcinogenic effects. 对苯ニ胺是染发等日化用品中ー种最常用的着色剂,由于其对人体的危害,近些年来被禁用或限用。 P ni amine is Dengri articles ー hair most commonly used coloring agents, due to the health hazards, in recent years are disabled or restricted. 作为日化产品卫生安全的瓶颈技术之一的标准物质纯度的測定,包括用高效液相色谱仪测定对苯ニ胺标准物质纯度时,对苯ニ胺标准物质纯度的溶液及其制备方法是标准物质纯度测定结果准确的关键因素。 Determination of purity of the substance of one of the health and safety of cosmetic products as a bottleneck, the amine includes p ni standard substance using HPLC purity analyzer, standard solution of the amine purity of the substance and preparation method is the standard p ni accurate results are a key factor in substance purity determination.

[0005] 现有技术采用高效液相色谱仪测定对苯ニ胺标准物质纯度时,是直接在色谱纯甲醇中加入对苯ニ胺标准物质制备成溶液,进行高效液相色谱检測。 [0005] the prior art when using high performance liquid chromatograph standard substance terephthalic ni amine purity, the amine is added p ni standard substance to prepare a solution, high performance liquid chromatography HPLC grade methanol directly. 由于对苯ニ胺很容易被空气中的氧气氧化,当未加入亚硫酸钠,且不控制温度时,高效液相色谱仪检测的色谱图很容易出现对苯ニ胺被氧化的峰,随着时间的推移,被氧化的峰越来越强,对苯ニ胺标准物质的峰越来越小。 Since p ni amines are easily oxidized by oxygen in the air, when no addition of sodium sulfite, and does not control the temperature, HPLC chromatograms detection is prone to be oxidized p ni amine peaks, as time transition, growing oxidation peaks, the amine p ni smaller peak standard substance. 而且溶液在30min内会改变颜色,从而导致高效液相色谱测定对苯ニ胺标准物质纯度结果不准确。 30min and the solution will change color, resulting in high performance liquid chromatography determination of the purity standard substance benzene ni amine inaccurate.

[0006] 发明内容 [0006] SUMMARY OF THE INVENTION

本发明所要解决的技术问题是提供一种能更加稳定、真实、精确的高效液相色谱仪測定对苯ニ胺标准物质纯度的溶液及其制备方法。 The present invention solves the technical problem is to provide a more stable solution of the amine purity standard substance and preparation method true, accurate HPLC determination of benzene ni. 本发明解决其技术问题采用的技术方案是:一种高效液相色谱仪测定对苯ニ胺标准物质纯度的溶液,它由色谱纯甲醇、浓度为l-lOPg/mL的亚硫酸钠和浓度为500-200(^g/mL的对苯ニ胺标准物质组成。在4-1 (TC的温度下,在色谱纯甲醇中依次添加亚硫酸钠和对苯ニ胺标准物质。本发明所要解决的技术问题还可进ー步通过如下技术方案加以解决:亚硫酸钠的浓度为lPg/mL、3Pg/mL、5Pg/mL、8Pg/mL 或10Pg/mL ;对苯ニ胺标准物质的浓度为500Pg/mL、800Pg/mL、1000Pg/mL、1500Pg/mL或200(^g/mL ;温度为4°C、6°C、8°C或10°C。本发明中的色谱纯甲醇为稀释液,用于稀释亚硫酸钠和对苯ニ胺标准物质,亚硫酸钠可减缓对苯ニ胺标准物质在空气中被氧化,对苯ニ胺标准物质用于计量量值溯源传递。本发明的色谱纯甲醇、亚硫酸钠和对苯ニ胺标准物质均可在中国国内市场购得。本发明由于采用上述 The present invention solves the technical problem using the technical solution is: A high performance liquid chromatography determination of the purity of aniline was ni standard substance, which was purified by chromatography pure methanol, at a concentration of l-lOPg / mL and sodium sulfite at a concentration of 500 200 (^ g / mL of benzyl amine ni standard substance. at a temperature of 4-1 (TC sequentially adding sodium sulfite and methanol in the chromatography ni amine terephthalic standard substance. the present invention solves the technical problem also into ー further be solved by the following technical solution: the concentration of sodium sulfite was lPg / mL, 3Pg / mL, 5Pg / mL, 8Pg / mL or 10Pg / mL; p ni amine concentration standard substance was 500Pg / mL, 800Pg / mL , 1000Pg / mL, 1500Pg / mL or 200 (^ g / mL;. a temperature of 4 ° C, 6 ° C, 8 ° C or 10 ° C in the present invention, chromatographic pure methanol as diluent used to dilute sodium sulfite and p ni amines standard substance, sodium sulfite can slow terephthalic ni amines standard substance is oxidized in the air, terephthalic ni amine standards for metering traceability transfer. HPLC grade methanol to the present invention, sodium sulfite, and p ni amine standard substances can be purchased in the Chinese domestic market. Since the present invention uses the above 术方案,减缓了对苯ニ胺被空气氧化的速度,且使对苯ニ胺标准物质的浓度为500-200(^g/mL,使得高效液相色谱仪能够准确、稳定的測定对苯ニ胺标准物质的纯度,确保了对苯ニ胺标准物质中的杂质均能被高效液相色谱仪检测,且不超过高效液相色谱仪检测的量程范围,有效地保障了日化用品中的有毒有害化学品检测工作的量值传递和安全卫生质量,防止了因相关物质超标而引发的贸易纠纷,提升了我国标准物质研制及在日化用品贸易监控中的优势,维护了我国的经济利益。 Program operation, by slowing the speed of the air oxidation of benzene amine ni, ni and p-phenylene amine concentration of the standard substance 500-200 (^ g / mL, so to be measured Gaoxiaoyexiang chromatography benzene ni accurately and stably with amine purity standard substance, to ensure that the standard substance terephthalic Ni amine impurities can be detected by high performance liquid chromatography, the range does not exceed the range of high performance liquid chromatography detection, effective protection of supplies toxic money transfer quality and safety and health hazardous chemicals detection work, preventing excessive due to related substances caused by trade disputes, enhance the development of reference materials and advantages of supplies trade monitoring, maintaining our country's economic interests.

附图说明[0007] 下面结合附图和本发明的具体实施例对本发明作进ー步详细描述: BRIEF DESCRIPTION [0007] Hereinafter, the present invention will be described in further detail in conjunction with the intake ー accompanying drawings and specific embodiments of the present invention:

图I是现有技术的色谱图。 Figure I is a chromatogram of the prior art.

[0008] 图2、图3、图4分别是本发明实施例2、实施例8、实施例10的色谱图。 [0008] FIGS. 2, 3, 4 are embodiments of the present invention Example 2, Example 8, Example 10 chromatogram.

[0009] 具体实施方式 [0009] DETAILED DESCRIPTION

_~!实施例I |卖施例2「实施例3丨实施例4 |卖施例5 _ ~ Example I |! Example 2 sell "Shu Example 3 Example 4 | Sell Example 5

色谱纯甲醇 IOOmL IOOmL IOOmL IOOmL IOOmL HPLC grade methanol IOOmL IOOmL IOOmL IOOmL IOOmL

亚硫酸纳 IOOKg 800Kg 500Kg 300Kg IOOOKg Sodium sulfite IOOKg 800Kg 500Kg 300Kg IOOOKg

对苯ニ胺标准物原booooc^g Ι80000μ8 I=IOOOOC^g [ΐ50000μ8 ]δ0000μ8 P ni standard primary amine booooc ^ g Ι80000μ8 I = IOOOOC ^ g [ΐ50000μ8] δ0000μ8

_1_实施例6 "!实施例7 1¾施例8 f实施例9 "!实施例10 _1_ Example 6! "Example 7 1¾ embodiments Example 9 Example 8 f"! Example 10

色谱纯甲醇 IOOmL : IOOmL IOOmL IOOmL IOOmL HPLC grade methanol IOOmL: IOOmL IOOmL IOOmL IOOmL

亚硫酸纳 IOOKg 800Kg 500Kg 300Kg IOOOKg Sodium sulfite IOOKg 800Kg 500Kg 300Kg IOOOKg

对苯ニ胺标准物原[50000μδ ]ΐ50000μ8 Ι80000μ8 I=IOOOOC^g ^OOOOC^g P ni standard primary amine [50000μδ] ΐ50000μ8 Ι80000μ8 I = IOOOOC ^ g ^ OOOOC ^ g

实施例11 :在4°C的温度下,在100 mL的色谱纯甲醇中依次添加IOOPg的亚硫酸钠和 Example 11: at a temperature of 4 ° C., Was added sequentially Add 100 mL of HPLC grade methanol and sodium sulfite IOOPg

200000μδ的对苯ニ胺标准物质。 Ni amine 200000μδ terephthalic standard substance.

[0010] 实施例12 :在60C的温度下,在100 mL的色谱纯甲醇中依次添加80(^g的亚硫酸钠和800(^g的对苯ニ胺标准物质。 [0010] Example 12: at a temperature of 60C, was added sequentially 80 (^ g of sodium sulfite and 800 (^ g of terephthalic standard substance ni amine Add 100 mL of HPLC grade methanol.

[0011] 实施例13 :在8°C的温度下,在100 mL的色谱纯甲醇中依次添加50(^g的亚硫酸钠和IOOOOOPg的对苯ニ胺标准物质。 [0011] Example 13: at a temperature of 8 ° C sequentially was added 50 (^ g sodium sulfite and amine IOOOOOPg terephthalic ni standard substance Add 100 mL of HPLC grade methanol.

[0012] 实施例14 :在10°C的温度下,在100 mL的色谱纯甲醇中依次添加30(^g的亚硫酸钠和15000(^g的对苯ニ胺标准物质。 [0012] Example 14: at a temperature of 10 ° C sequentially was added 30 (^ g sodium sulfite and 15000 (^ g of terephthalic standard substance ni amine Add 100 mL of HPLC grade methanol.

[0013] 实施例15 :在10°C的温度下,在100 mL的色谱纯甲醇中依次添加IOOOPg的亚硫酸钠和5000(^g的对苯ニ胺标准物质。 [0013] Example 15: at a temperature of 10 ° C sequentially added IOOOPg sodium sulfite and 5000 (^ g of terephthalic standard substance ni amine Add 100 mL of HPLC grade methanol.

[0014] 实施例16 :在4°C的温度下,在100 mL的色谱纯甲醇中依次添加IOOPg的亚硫酸钠和5000(^g的对苯ニ胺标准物质。 [0014] Example 16: at a temperature of 4 ° C., Was added successively sodium sulfite and IOOPg 5000 (^ g of terephthalic standard substance ni amine Add 100 mL of HPLC grade methanol.

[0015] 实施例17 :在6°C的温度下,在100 mL的色谱纯甲醇中依次添加80(^g的亚硫酸钠和15000(^g的对苯ニ胺标准物质。 [0015] Example 17: at a temperature of 6 ° C, was added sequentially 80 (^ g sodium sulfite and 15000 (^ g of terephthalic standard substance ni amine Add 100 mL of HPLC grade methanol.

[0016] 实施例18 :在8°C的温度下,在100 mL的色谱纯甲醇中依次添加50(^g的亚硫酸钠和8000(^g的对苯ニ胺标准物质。[0017] 实施例19 :在10°C的温度下,在100 mL的色谱纯甲醇中依次添加30(^g的亚硫酸钠和IOOOOOPg的对苯ニ胺标准物质。 [0016] Example 18: at a temperature of 8 ° C sequentially was added 50 (^ g of sodium sulfite and 8000 (^ g of terephthalic ni amines standard substance Add 100 mL of HPLC grade methanol [0017] Example 19. : at a temperature of 10 ° C, was added 30 (^ g sodium sulfite and amine IOOOOOPg terephthalic ni standard substance sequentially Add 100 mL of HPLC grade methanol.

[0018] 实施例20 :在10°C的温度下,在100 mL的色谱纯甲醇中依次添加IOOOPg的亚硫酸钠和20000(^g的对苯ニ胺标准物质。 [0018] Example 20: at a temperature of 10 ° C sequentially was added sodium sulfite and IOOOPg 20000 (^ g of terephthalic standard substance ni amine Add 100 mL of HPLC grade methanol.

[0019] 上述产品实施例I 一10分别对应于方法实施例11 一20。 Example I [0019] 10 one embodiment of the above product in Example 11 respectively corresponding to a 20 method embodiment.

Claims (5)

1. 一种高效液相色谱仪测定对苯ニ胺标准物质纯度的溶液,其特征是:它由色谱纯甲醇、浓度为l-lOPg/mL的亚硫酸钠和浓度为500-200(^g/mL的对苯ニ胺标准物质组成。 An HPLC determination of purity of the aniline was ni standard substance, characterized in that: it consists of chromatographically pure methanol, at a concentration of l-lOPg / mL and sodium sulfite at a concentration of 500-200 (^ g / mL ni amine terephthalic standard substance.
2.根据权利要求I所述的ー种高效液相色谱仪测定对苯ニ胺标准物质纯度的溶液,其特征是:亚硫酸钠的浓度为lM€/mL、3Pg/mL、5Pg/mL、8Pg/mL或10Pg/mL。 The high performance liquid chromatograph ー I according to claim amine purity standard substance solution terephthalic ni, characterized in that: the concentration of sodium sulfite was lM € / mL, 3Pg / mL, 5Pg / mL, 8Pg / mL or 10Pg / mL.
3.根据权利要求I所述的ー种高效液相色谱仪测定对苯ニ胺标准物质纯度的溶液,其特征是:对苯ニ胺标准物质的浓度为50(^g/mL、80(^g/mL、lOOOPg/mL、150(^g/mL或2000M<g/mL。 The HPLC assay ー species I according to claim purity terephthalic standard substance solution of the amine ni, wherein: p ni standard substance concentration of the amine is 50 (^ g / mL, 80 (^ g / mL, lOOOPg / mL, 150 (^ g / mL or 2000M <g / mL.
4. 一种如权利要求I所述的高效液相色谱仪测定对苯ニ胺标准物质纯度的溶液制备方法,其特征是:在4-10°C的温度下,在色谱纯甲醇中依次添加亚硫酸钠和对苯ニ胺标准物质。 I 4. A claim according to HPLC determination of the amine solution preparation method ni benzene purity standard substance, wherein: at a temperature of 4-10 ° C are sequentially added methanol chromatography sodium sulfite and material standards terephthalic ni amine.
5.根据权利要求4所述的ー种溶液制备方法,其特征是:温度为4°C、6°C、8°C或10°C。 5. Preparation of 4 ー method according to claim solution, characterized in that: a temperature of 4 ° C, 6 ° C, 8 ° C or 10 ° C.
CN201210106235XA 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 CN102680592A (en)

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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

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* Cited by examiner, † Cited by third party
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

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* Cited by examiner, † Cited by third party
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》 *
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