化妆品中重金属含量测定

1、黑龙江东方学院本 科 生 毕 业 论 文（设 计）The Determination of Heavy Metals in Cosmetics 化妆品中重金属含量的测定学生姓名 赵 红 学 号 054131233 专 业 食品科学与工程 班 级 2005C 指导教师 杨同舟 张寒冰 学 部 食品与环境工程学部 答辩日期 2009年5月24日 黑龙江东方学院本科生毕业论文（设计）The determination of heavy metals inCosmetics AbstractCosmetics impose on the surface of the body, play a role

2、 of clean, maintenance, landscaping and removal the bad smell. However, in the course of the production of cosmetics , the raw materials or intermediate inputs can be mixed with a number of restricted substances, in order to understand and master its limit value of the quality of the material, that

3、is to do an analysis of physical and chemical indicators. In this paper, trace elements of arsenic and lead are determined by microwave digestion / inductively coupled plasma mass spectrometry in the cosmetics, the method has the advantages a short time, less consumption of reagents, loss of a small

4、 element, accurate measurement, Trace elements of mercury was determined by direct determination of mercury analyzer, the method is simple, sensitive, safe, fast, time-saving.The results are as follows:Hong Kong Monetary olary Cosmetics Co., Ltd. produce Xue Yan lasting whitening liquid foundation,

5、Hong Kong Monetary olary Cosmetics Co., Ltd. produce Xue Yan Whitening Moisturizer，Shenzhen Green Xin Daily Cosmetics Co., Ltd. produce eight glasses of water nutrition moisturizing cream, Johnson & Johnson (China) Co., Ltd. produce Johnson & Johnson baby nourishing moisture: the content of lead wer

6、e1.244mg/kg、0.042 mg/kg、0.046mg/kg、0.339mg/kg；the content of mercury were 0.1013 mg/kg、0.0974mg/kg、0.0625mg/kg、0.0193mg/kg； the content of arsenic content were 0.345 mg/kg、0.037 mg/kg、0.127 mg/kg、0.036 mg/kg；the three kinds heavy metals in Cream Cosmetics were limited : the lead (lead in total) 40mg

7、/kg, mercury 1mg/kg, arsenic (arsenic in total) 10mg/kg. The results show that the three kinds of heavy metals detected in cosmetics are not exceeded.Keywords： cosmetics ；the content of heavy metal ；Microwave digestion / inductively coupled plasma mass spectrometry化妆品中重金属含量的测定摘 要化妆品施于人体表面,起到清洁,保养,美化

8、或清除不良气味的作用。但在生产化妆品的过程中,所投入的原料或中间体均可混入一些限用的物质,为了解和掌握其限用物质的质量值,即做某些理化指标的分析。本文中微量元素铅，砷的测定采用微波消解/电感耦合等离子质谱仪的方法测定一些市售化妆品中的微量元素铅，砷的含量，该方法具有时间短，消耗试剂少，元素损失少测定的结果准确率高等优点。微量元素汞的测定采用测汞仪直接测定，该方法具有操作简单，灵敏度高，安全，快速，省时等优点。测定结果如下：香港金欧莱化妆品有限公司生产的雪颜美白持久粉底液，香港金欧莱化妆品有限公司生产的雪颜美白保湿乳液，深圳市绿馨日用化妆品有限公司生产的八杯水营养保湿霜，强生（中国）有限公司生产

9、的强生婴儿保湿滋润霜，铅的含量分别为1.244mg/kg、0.042 mg/kg、0.046 mg/kg、0.339 mg/kg；汞的含量分别为0.1013 mg/kg、0.0974 mg/kg、0.0625 mg/kg、0.0193 mg/kg；砷的含量分别为0.345 mg/kg、0.037 mg/kg、0.127 mg/kg、0.036 mg/kg。铅、砷、汞3种重金属元素在膏霜类化妆品中的限量分别为铅（以铅计）40 mg/kg，汞1 mg/kg，砷（以砷计）10 mg/kg。结果显示四种化妆品中检测的重金属均不超标。关键词：化妆品 ; 重金属 ; 含量微波消解/电感耦合等离子质谱仪15

10、黑龙江东方学院本科生毕业论文（设计）ContentsAbstract in EnglishiAbstract in ChineseiiChapter 1 Introduction11.1 The purpose and significance of detection in this paper11.2 Common detection methods of cosmetics21.3 The hazards of heavy metals in cosmetics41.3.1 The hazards of mercury and its compounds41.3.2 The hazard

11、s of arsenic and its compounds51.3.3 The hazards of lead and its compounds5Chapter 2 Materials and Methods72.1 Experimental materials72.2 Instruments and reagents72.3 Methods and procedures82.3.1 Sample pre-treatment8 2.3.2 The determination of lead in cosmetics82.3.3 The determination of arsenic in

12、 cosmetics92.3.4 The determination of mercury in cosmetics9Chapter 3 Results and Analysis103.1 The results and analysis of lead content in four kind of cosmetics103.2 The results and analysis of mercury content in four kind of cosmetics113.3 The results and analysis of arsenic content in four kind o

13、f cosmetics11Conclusions12References14Acknowledgements15Chapter 1 Introduction 1.1 The purpose and significance of this paperWith the development of our society, cosmetics have become people daily life an indispensable element, in order to ensure that there is no harmful because of the use of cosmet

14、ics to consumers, many countries have formulated laws and regulations to manage cosmetics. raw materials, finished products of cosmetics to carry out a strict requirement. Chinas legal system and supervision of the Ministry of Health Division of Health has also formulated a Hygienic Standard for Cos

15、metics, provides raw materials and cosmetic hygiene requirements of the final product. Countries implement health monitoring system. Health administrative departments of the State Council in charge of the national health supervision of cosmetic products, local peoples governments above the county le

16、vel health administrative departments in charge of this area of the health supervision of cosmetic products 1.Recent years, Chinas sustained economic development and peoples consumption levels a significant increase in skin-care beauty of daily life has become an indispensable necessity, the functio

17、n of cosmetics is now gradually modified by the simple beauty to the functional aspects extension, there are many types of cosmetics for special purposes. various brands of sunscreen, speckle reducing, wrinkle reduction phytosome, tender skin whitening and other cosmetic products in the domestic mar

18、ket has emerged.Access to the rapid development of cosmetic industry, the sales increase, the adverse reactions caused by cosmetics from time to time, consumers greatly enhance the safety awareness, hair dye allergy, freckle whitening products are often reported the content of heavy metals are excee

19、ded, in particular in cosmetics banned substances were detected shocked the world, these problems reflect the safety of cosmetic products , due to the existence of these problems, consumers should have a more objective understanding of science Lead, mercury, arsenic is highly toxic accumulation of h

20、armful elements, belonging to banned substances in cosmetics , Them is not permitted to add man-made, but in the course of the production of a number of cosmetics use raw materials itself contains a small amount of lead, mercury, arsenic, in order to achieve the purpose of antibacterial, antimicrobi

21、al, and whitening, result in a significant increase of heavy metals in cosmetics, so the national standard for lead, mercury, arsenic and other toxic substances have made clearly regulate, cosmetics norms of the National Health will review the provisions of health projects 2, Hygienic Standards for

22、Cosmetics is a national mandatory standards, toxic and harmful elements of its provisions made. Toxic and harmful elements: standards set forth in the mercury , arsenic and lead in the cream cosmetics limited.mercury 1mg/kg 3, arsenic (arsenic in total) 10mg/kg 4, lead (lead in total) 40mg/kg 5, The

23、 three kinds of heavy metal elements which comes mainly from the impact of human activities affected the environment, including soil pollution, river pollution and the introduction of raw materials pollution, lead, arsenic and mercury are harmful to human health 6, so that their content in cosmetics

24、 should be lower. Under the existing standard test of these projects has become a necessity of life, increasing sales volume, product brands, increasing the number of varieties. Cosmetics safety and health are closely related to peoples health , because of heavy metals in the special purpose of bein

25、g used for cosmetics, but their harm to the human body is well known ,some of the material has a strong toxicity, mutagenicity, carcinogenicity, teratogenicity, what is more on the skin and mucous membrane may cause obvious damage, the heavy metal content in cosmetics is one of the indicators will b

26、e detected7.1.2 Common detection methods of cosmeticsCosmetics chemical standard test method provides test cosmetics are mainly high-performance liquid chromatography flame atomic absorption spectrometry, atomic fluorescence wet digestion and microwave digestion ICP-MS (inductively coupled plasma ma

27、ss spectrometry, ICP-MS ). 8 High Performance Liquid Chromatography (HPLC) for short also known as high-pressure or high-speed liquid chromatography, high performance liquid chromatography separation or modern column chromatography to liquid as the mobile phase, using high-pressure fluid system, is

28、color spectrum of an important branch of law. It is made of high-pressure pump will have a different polarity, the ratio of a single solvent or a mixture of different solvents, such as the mobile phase buffer with a fixed phase pumped into the column, the injection valve into the sample by the mobil

29、e phase with into the column in the column after the separation of the components were, in order to enter the detector test in order to achieve the analysis of samples. This method has become a chemistry,biochemistry, medicine, industry, agriculture, environmental protection, inspection and seizure

30、law in important areas such as the separation and analysis technology, analytical chemistry, biochemistry and environmental chemistry of the essential tools the hands of workers.Atomic absorption spectrophotometry, it is a test element from the hollow cathode lamp to emit a certain intensity and spe

31、ctral characteristics of a certain wavelength of light, when it contains a test element through the ground state of the flame atomic vapor when some of the characteristics of the light spectrum is absorbed, and not absorption of light by the monochromator, the photoelectric detector exposure was det

32、ected, according to the characteristics of light absorption spectrum of the extent, it will test measured like elements in the test.Wet digestion atomic fluorescence spectrometry ，it is that high-pressure sealed using PTFE digestion Couplers can sample digestion products will be transferred to diges

33、t a good sample of 10mL bottle volume, deionized water volume 10mL, shaken. 1.0mL injection cold vapor atomic fluorescence in the detector response to the bottle, adding 0.2mL10% SnCl2, goods Couplers solution SnCl2 trace mercury has been reduced to mercury vapor, mercury vapor by argon gas into the

34、 fluorescence chamber, resulting in fluorescence. Determination of this method time is short digestion, the volatile loss of mercury-free, less interference, lower detection limit for (100ng / L), recovery rate of 95.7% -98.0%, good reproducibility, relative standard deviation of 2.6%.Microwave Dige

35、stion Inductively Coupled Plasma Mass Spectrometry,It is nitric acid and hydrogen peroxide pretreatment solution of cosmetics, the role of the electric field in the microwave the next, so that high-speed molecular friction and collisions, microwave energy to thermal energy. Conditions in the heating

36、, due to acid oxidation and increase in activity, making cosmetics in a relatively short time period , so cosmetics lead, arsenic, mercury ion in the state will exist in the test solution 9. Microwave digestion is a highly effective method of sample handling, it has a fast decomposition of samples w

37、ith good accuracy and precision, high sensitivity, elements not easily measured, as well as blank and low losses, currently at home and abroad, has been widely used in cosmetics , pharmaceuticals, plastic products such as pre-treatment samples. The method of cosmetic products of lead, arsenic treatm

38、ent of samples with good results, and a resolution to be detected in a variety of elements in cosmetics, the digestion method is simple, time short, less reagent consumption, high accuracy measurements of the characteristics of an ideal sample preparation is one of the ways, lead, arsenic determinat

39、ion by carrier gas to the sample directly into apparatus, does not require any preconcentration, separation step, direct determination of high sensitivity, small interference.Inductively coupled plasma mass spectrometry is based on inductively coupled plasma (ICP) ionization source for mass spectrom

40、etry analysis. It has high sensitivity, simple lines, linear dynamic range, can be multi-element detection , At the same time, It is a potential multi-element and isotope ratio analysis, has been widely used in environmental, metallurgical, oil, , medical, semiconductor, and other fields of nuclear

41、materials analysis. ICP-MS from the power source is inductively coupled plasma (ICP), the main is a three-tier, composed of quartz torch casing pipe, tube top around the torch has load coils, the sample from the carrier gas into the plasma torch flame will occurrence of evaporation, decomposition, e

42、xcitation and ionization, auxiliary gas used to maintain the plasma. Tangent direction of cooling air to the introduction of outer tube, resulting in a spiral flow to the load coil outside the tube wall to be cooled. The most common way is to use sampling or right-angle type concentric pneumatic neb

43、ulizer generated aerosols, taken off the set in the carrier gas is injected into flame torch, the sample injection volume of about 1ml/min, by peristaltic pump into the fog of devices. At about 10mm above the load coil, the torch flame temperature of about 8000K, in such a high temperature, the ioni

44、zation energy of the elements below 7eV fully ionized, the ionization energy below the ionization degree of the elements 10.5ev greater than 20%. As the most important element in ionization energy is lower than 10.5eV, therefore have a very high sensitivity 10.1.3 The hazards of heavy metals in cosm

45、etics In modern society, the use of lipstick, skin care, sunscreen, whitening beauty cream, hair dye and other cosmetics is more and more , sustainable use of cosmetics for nearly decades. A significant portion of the above cosmetics (including some of the worlds leading brands) contain different le

46、vels of heavy metals . These have been detected or have not been detected . the harmful ingredients, the body will absorb some or all of them , at last deposition in the blood or organ cells of the human body, they will be a bomb hidden in the body, may endanger the physical health 11. Let us unders

47、tand the risks of heavy metals:1.3.1 The hazards of mercury and its compounds Mercury and its compounds were banned in cosmetic, Them exist as impurities the limit is less than 1mg/kg. However, In view of sulphide of mercury (ethyl mercury thio sodium salicylate) with the purpose of good inhibitory

48、effect, allowing for eye make-up and eye make-up remover products, HgS pigment is generally added to the red lipstick, color cosmetics such as rouge, mercuric chloride used in cosmetics with the purpose of white, delicate, mercury ions can interfere with human skin in the process of tyrosine into me

49、lanin, are generally added in the whitening, whitening, speckle reducing cosmetics, low prices of these substances, so HgS, mercuric chloride and even the use of modern cosmetics maker 13. Mercury and its compounds can pass through the skin barrier into the body all the organs and tissues, mainly th

50、e most damage to the kidneys, followed by the liver and spleen, destruction of enzyme system activity, so that protein coagulation, tissue necrosis, with marked gonadal toxicity, embryo drug and the role of cell genetics. Chronic toxicity of mercury and its compounds as the main clinical manifestati

51、ons: fatigue, weakness, drowsiness, apathy, emotional instability, headache, dizziness, tremor, as well as hemoglobin and red blood cell, WBC reduction ,liver damage and so on, in addition to sensory peripheral receded, concentric narrowing the field of vision, hearing impairment and the Masonic mov

52、ement disorders and so on12.1.3.2 The hazards of arsenic and its compounds Arsenic and its compounds in components of cosmetics for the prohibited substances , they are widespread in nature, cosmetic raw material and cosmetics production process, also vulnerable to arsenic contamination, so as the e

53、xistence of impurities, arsenic in cosmetics for the limits is less than 10mg/kg (arsenic in total) 13. Arsenic and its compounds are considered carcinogens, long-term use cosmetics with high arsenic can cause dermatitis, skin pigmentation, eventually leading to skin cancer. Arsenic and its compound

54、s as the main clinical manifestations poisoning peripheral neuritis symptoms such as pain in the limbs, difficulty walking, muscle atrophy, brittle hair easy to fall off, skin pigment a high degree of calm, the palm of your hand a high degree of foot plantar keratosis skin, repeat-like hyperplasia,

55、chapped, ulcers enduring, you can change skin of skin cancer and may die from complications. If cosmetics added excessive arsenic poisoning after use, then if the absorption, arsenic can lead to changes in the nervous system, at the same time there are some changes in peripheral nerves, such as limb

56、s rigid body weakness, pain and other symptoms, There may be changes skin on the black, pigments calm.1.3.3 The hazards of lead and its compounds Lead and its compounds in components of cosmetics for the prohibited substances , as the impurity element content in cosmetics should not exceed 40mg/kg (

57、lead in total) . Lead in cosmetics can increase the skins white , it is added to whitening, whitening cosmetics. All the biological effect of lead on both toxic. Lead and its compounds absorbed through the skin and harm to human health, mainly affecting the nervous system, kidneys, gastrointestinal

58、tract, reproductive function, cardiovascular, immune and endocrine systems, particularly affect fetal health. The main clinical manifestations central nervous system function as a result of disorder arising from neurasthenia syndrome. Acute or subacute encephalopathy. Ataxia. The loss of appetite , metallic taste in the mouth, gingival lead line, abdominal cramps, nausea, vomiting, diarrhea. Hematopoietic sys