【作者】 刘海艳；

【导师】 王英华；

【作者基本信息】 吉林大学 ， 分析化学， 2010， 硕士

【摘要】 金樱子棕和胭脂虫红两种食品添加剂在食品加工过程中作为着色剂使用,目前我国尚无质量检验方法标准,这给金樱子棕和胭脂虫红两种食品添加剂的生产使用和进出口贸易以及食品卫生监测工作带来很大的困难。为了保证进出口食品添加剂金樱子棕和胭脂虫红产品质量和使用安全,维护消费者的利益,需要尽快制定相应的质量检验标准,以便指导相关企业生产、改进生成工艺、加强生产管理,保证上述两种食品添加剂的产品质量和进出口贸易工作的顺利进行,因此制定进出口食品添加剂金樱子棕和胭脂虫红的质量检验标准和相应的检测方法有着重要的意义。本文主要研究了金樱子棕和胭脂虫红两种食品着色剂的质量检测方法,并确定了主要质量指标,包括纯度(或含量)、干燥失重、灼烧残渣、重金属杂质铅和砷以及相应的检测方法。应用紫外可见分光光度法测定金樱子棕和胭脂虫红的纯度(或含量),采用一定浓度的金樱子棕溶液的吸光度值间接测定其纯度,解决了金樱子棕在紫外可见区没有特征吸收无法测试的难题;深入研究了石墨炉原子吸收法测定杂质铅时的灰化温度、原子化温度和基体改进剂等实验条件,研究了原子荧光光度法测定杂质砷时的灯电流、负高压、原子化器高度、载气流量、硼氢化钾浓度等实验条件,建立了测定金樱子棕和胭脂虫红中杂质铅和砷的测定方法和质量标准;采用重量法检测了金樱子棕和胭脂虫红的干燥失重和灼烧残渣,确定了相应的质量标准。本文研究成果经国内相关单位的验证,根据相关文献和我国的实际情况,确立了金樱子棕和胭脂虫红两种食品添加剂的质量标准的主要质量指标和检测方法,为国家质检总局制定相关的国家标准提供了可靠的依据。2009年10月,依据此项目的研究成果所拟定的金樱子棕和胭脂虫红国家标准已经通过中华人民共和国国家质量监督检疫总局的审批。更多还原

【Abstract】 The establishment of quality standards is in order to ensure the safeties of food additives for import and export, ensure the quality of food additives, safeguard the interests of consumers. The quality standards can guidance production related to business, improve produced technology, strengthen production management, ensure the smooth implement of import and export trade, and improve the international competitiveness of China’s food additives. The establishment of quality standards for food additives is in line with national conditions, urgent matters, and national quality standards for food additives are very important for the formulation of the guidance and supervision.Rosa laevigata michx brown and Carmine were allowed to use as food additives in the country, and used as colorants which are natural and edible.“Use and health Standards of Food Additive”only gives the scope of use and use limited. Rosa laevigata michx brown has no relevant international standards. Carmine has the food additive standards which are slightly different in the JECFA law and FCC, but there are not corresponding quality standards of Rosa laevigata michx brown and Carmine in the country. There is urgent to establish quality standards of Rosa laevigata michx brown and Carmine to ensure effective implementation of inspection and quarantine on import and export and monitor product quality.The content of this paper is to build quality standards of Rosa laevigata michx brown and Carmine, to set their main quality indicators, and to study corresponding detection methods. Quality indicators contain purity or content, dry weight loss, residue on ignition, heavy metals lead and arsenic. UV visible spectrometry was used to determine the purity or content; in different temperature, constant weight methods are used to determine dry weight loss and residue on ignition; lead is determined by graphite furnace atomic absorption spectrometry; arsenic is determined by atomic fluorescence spectrometry.In this paper, not only identification tests of Rosa laevigata michx brown and Carmine were carried out, but also more conditions including ash temperature, atomization temperature and the matrix of experimental conditions to improve agent were studied using graphite furnace atomic absorption. The experimental conditions of atomic fluorescence spectrophotometer are discussed, which contain lamp current, negative pressure, atomizer height, flow of carrier gas, concentration of carrier and concentration of potassium borohydride.The determination results of Rosa laevigata michx brown as follows: The absorbance of a 1% Rosa laevigata michx brown of Lianyi biology solution was 0.41; Loss on drying was 2.68%; Loss on ignition was 8.49%; Lead was determined by graphite furnace atomic absorption spectrometry, and the content was 0.076 mg / kg; Arsenic was determined by atomic fluorescence spectrometry, and the content was 0.182 mg / kg. The absorbance of 1% solution of Changyue Zhihua was 0.45; Loss on drying was 4.93%; Loss on ignition was 2.88%; The content of lead was 0.111 mg / kg, the recovery of lead was 82.5%～96.0%; The content of arsenic was 0.263 mg / kg, the recovery of arsenic was 80.5 ~ 105.8%.The determination results of Carmine as follows: The content of carmine acid in sample 1 (Qingdao Dehui Corporation)was 51.41% and sample 2 (Qingdao Dehui Corporation) was 51.32%; The content of carmine acid in Sigma company sample was 55.02%; Loss on drying of sample 1 was 10.12% and the sample 2 was 6.13%; Lead in sample 1 was determined by graphite furnace atomic absorption spectrometry, the content was 0.55 mg / kg and the recovery was 97.0% ~ 107.8%; Arsenic in sample 1 was determined by atomic fluorescence spectrometry, the content was 0.151 mg / kg and the recovery was 86.8% ~ 103.4%. In the condition of 920℃, the residue on ignition of sample 1 was 13.46%. The residue on ignition in sample of Shantou Mingde Corporation was 17.30%.Based on the literature, experimental data and verify the relevant units, eventually quality indicators established of Rosa laevigata michx brown and Carmine are as follows:Rosa laevigata brown’s main technical specifications are: absorbance is not less than 0.35; loss on drying is not more than 5.0%; residue on ignition is not more than 10.0%; lead is not more than 2.0 mg / kg; arsenic is not more than 1.0 mg / kg. The main technical specifications of Carmine are: the content of carmine acid is not less than 50.0%; loss on drying is not more than 20.0%; residue on ignition is not more than 18.0%; lead is not more than 2.0 mg / kg; arsenic shall not be greater than 1.0 mg / kg.The study results of this paper:(1) Solve difficult quantitative problems of Rosa laevigata michx brown. Substance of showing Color of Rosa laevigata michx brown is a mixture including many pigments. It is difficult to find a single color component to determine quantificationally. Colored solution of Rosa laevigata michx brown has light absorption of light, which can indirectly express color components. Rosa laevigata michx brown no characteristic absorption in the ultraviolet region and visible light region. According to the standards of similar colorants and experimental conditions, the absorbance of 1% solution chosen of Rosa laevigata michx brown was determined at 580 nm.(2) Solve the problem of residue on ignition for Carmine. The experimental results of ash and residue at 800℃were higher. According to documents, Merkel light was needed to measure residue. Muffle furnace can get the requested temperature of Merkel light (flame temperature of 900℃~920℃) in China’s actual conditions. Residues on ignition in the Carmine samples of Qingdao Dehui and Shandou Mingde were determined at 920℃and the results were higher than requirement of FCC. In the end, the indicator of residues on ignition was built according to the experimental data and the practical application.(3) Solve the problem of lower recovery rate when lead was determined in Carmine. The lower recovery rate appeared because Carmine contains many metal elements such as aluminum. The standard addition method was used to determine the content of lead in Carmine, which can overcome the interference of other elements and ensure the accuracies of recovery and test.The establishment of national quality standards which were the two kinds of colorants of Rosa laevigata michx brown and Carmine provided the guarantee and accordance to ensure product quality and the trade of import and export. It was consistent with national conditions and needs. It filled the domestic blank, ensured the quality of food additives and safeguarded the interests of consumers.It was favored to guidance production related to business, improve produced technology, strengthen production management.In 2009, the research results of national standards for Rosa laevigata michx brown and Carmine has been adopted by The People’s Republic of China General Administration of Quality Supervision and Quarantine, awaiting enactment.更多还原