保健食品中主要化学危害物质检测技术研究

发布时间：2018-01-18 03:12

本文关键词：保健食品中主要化学危害物质检测技术研究　出处：《浙江海洋大学》2017年硕士论文　论文类型：学位论文

【摘要】：本研究通过试验优化设计,建立了针对保健食品中主要化学危害物质(多残留农药、非法添加雌激素化学药物)的检测方法,为相关部门标准制定,净化保健食品市场提供一定的数据支持。具体工作内容如下:1、通过对87批次的铁皮石斛、灵芝孢子粉、蜂胶、珍珠粉等保健食品原料中可能存在的敌敌畏、久效磷、甲拌磷、乐果、甲基对硫磷、甲基嘧啶磷、毒死蜱、马拉硫磷、倍硫磷等9种农药残留进行风险监测,并提出监管建议。本研究结果表明,灵芝提取物中检出毒死蜱和敌敌畏,含量分别为0.075 mg/kg、0.033 mg/kg,西洋参中检出毒死蜱含量为0.031 mg/kg,其他批次均未检出上述农药残留。针对检测结果进行原因分析并提出监管建议。2、通过气相色谱及质谱条件的优化,标准溶液溶剂选择、基质效应考察及QuEChERS法和FaPEx法两种前处理方式的比较,最终建立了FaPEx柱快速萃取净化-GC/MS/MS同时检测保健食品原料中多残留农药的方法体系。该方法(体系)下,95种农药化合物在一定浓度范围内存在良好的线性关系,相关系数均大于0.99,定量限在0.001~0.150 mg/kg。100 ng/mL时除百菌清未检出,其他94种农药化合物的平均加标回收率(Rec)为65.7%~156.0%,相对标准偏差(RSD)为0.3%~15.4%。该方法在保证较好检测结果准确度的前提下,可有效去除杂质,减少对仪器的污染程度,延长仪器使用寿命;同时,该方法大大缩短了前处理时间,减少了有机溶剂的使用量,为保健食品原料中多农药残留检测提供了一定的参考意义。3、通过液相色谱及质谱条件的优化,提取溶剂的选择,最终建立了美容养颜类保健食品中非法添加9种雌激素的LC-MS/MS方法,其在一定浓度范围内线性关系良好,其相关系数为0.9980~0.9999,检出限为2.3~23.1 mg/kg。低、中、高三个浓度水平下平均加标回收率(Rec)为84.65%~109.86%,相对标准偏差(RSD)为7.32%~14.72%,表现为良好的准确度和精密度。
[Abstract]:This study through the experiment optimization design, is established according to the main chemical hazards in health food (pesticide residue, chemical drugs added illegally estrogen) detection method for the formulation of relevant departments, purify the health food market to provide some data to support. The specific contents are as follows: 1, based on 87 batches of Dendrobium officinale, Ganoderma lucidum spore powder, propolis, dichlorvos may exist pearl powder health food raw materials, monocrotophos, phorate, dimethoate, methyl parathion, pirimiphos methyl, chlorpyrifos, malathion, risk monitoring residues of 9 pesticides fenthion, and put forward suggestions. The research results showed that chlorpyrifos and dichlorvos were detected in extracts of Ganoderma lucidum in the content were 0.075 mg/kg, 0.033 mg/kg, American ginseng in detection of chlorpyrifos content was 0.031 mg/kg, other batches were not detected. The detection results for pesticide residues Reason analysis and put forward the suggestion of supervision.2, optimized by gas chromatography and mass spectrometry conditions, standard solution, solvent selection, comparative study of matrix effects and QuEChERS method and FaPEx method two kinds of pretreatment methods, finally established the FaPEx -GC/MS/MS column rapid extraction purification method for simultaneously detecting system of pesticide residues in the raw materials of health food. (system), 95 kinds of pesticide compounds in a certain concentration range of memory in a good linear relationship, the correlation coefficients were greater than 0.99, the limit of quantification in 0.001~0.150 mg/kg.100 ng/mL in chlorothalonil was not detected, the other 94 kinds of pesticide compounds, the average recoveries (Rec) for 65.7%~156.0%, the relative standard deviation (RSD) 0.3%~15.4%. is the method to ensure better detection results of the same accuracy, can effectively remove impurities, reduce the degree of pollution of the equipment, prolong the service life of the instrument; at the same time, this method greatly reduced The processing time, reduce the amount of organic solvent,.3 detection provides some reference for the health food raw materials in pesticide residues, optimized by liquid chromatography and mass spectrometry conditions, extraction solvent selection, finally established the LC-MS/MS method to add non law beauty foods in 9 kinds of estrogen. In a certain concentration range a good linear relationship, the correlation coefficient is 0.9980~0.9999, the detection limit is 2.3~23.1 mg/kg. low, high levels of the average recoveries (Rec) for 84.65%~109.86%, the relative standard deviation (RSD) of 7.32%~14.72%, showed good accuracy and precision.

【学位授予单位】：浙江海洋大学
【学位级别】：硕士
【学位授予年份】：2017
【分类号】：O657.63;TS218

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