本文關(guān)鍵詞：保健食品中主要化學危害物質(zhì)檢測技術(shù)研究　出處：《浙江海洋大學》2017年碩士論文　論文類型：學位論文

  更多相關(guān)文章： 保健食品 農(nóng)藥殘留 雌激素 LC-MS/MS GC/MS/MS FaPEx

【摘要】：本研究通過試驗優(yōu)化設(shè)計,建立了針對保健食品中主要化學危害物質(zhì)(多殘留農(nóng)藥、非法添加雌激素化學藥物)的檢測方法,為相關(guān)部門標準制定,凈化保健食品市場提供一定的數(shù)據(jù)支持。具體工作內(nèi)容如下:1、通過對87批次的鐵皮石斛、靈芝孢子粉、蜂膠、珍珠粉等保健食品原料中可能存在的敵敵畏、久效磷、甲拌磷、樂果、甲基對硫磷、甲基嘧啶磷、毒死蜱、馬拉硫磷、倍硫磷等9種農(nóng)藥殘留進行風險監(jiān)測,并提出監(jiān)管建議。本研究結(jié)果表明,靈芝提取物中檢出毒死蜱和敵敵畏,含量分別為0.075 mg/kg、0.033 mg/kg,西洋參中檢出毒死蜱含量為0.031 mg/kg,其他批次均未檢出上述農(nóng)藥殘留。針對檢測結(jié)果進行原因分析并提出監(jiān)管建議。2、通過氣相色譜及質(zhì)譜條件的優(yōu)化,標準溶液溶劑選擇、基質(zhì)效應(yīng)考察及QuEChERS法和FaPEx法兩種前處理方式的比較,最終建立了FaPEx柱快速萃取凈化-GC/MS/MS同時檢測保健食品原料中多殘留農(nóng)藥的方法體系。該方法(體系)下,95種農(nóng)藥化合物在一定濃度范圍內(nèi)存在良好的線性關(guān)系,相關(guān)系數(shù)均大于0.99,定量限在0.001~0.150 mg/kg。100 ng/mL時除百菌清未檢出,其他94種農(nóng)藥化合物的平均加標回收率(Rec)為65.7%~156.0%,相對標準偏差(RSD)為0.3%~15.4%。該方法在保證較好檢測結(jié)果準確度的前提下,可有效去除雜質(zhì),減少對儀器的污染程度,延長儀器使用壽命;同時,該方法大大縮短了前處理時間,減少了有機溶劑的使用量,為保健食品原料中多農(nóng)藥殘留檢測提供了一定的參考意義。3、通過液相色譜及質(zhì)譜條件的優(yōu)化,提取溶劑的選擇,最終建立了美容養(yǎng)顏類保健食品中非法添加9種雌激素的LC-MS/MS方法,其在一定濃度范圍內(nèi)線性關(guān)系良好,其相關(guān)系數(shù)為0.9980~0.9999,檢出限為2.3~23.1 mg/kg。低、中、高三個濃度水平下平均加標回收率(Rec)為84.65%~109.86%,相對標準偏差(RSD)為7.32%~14.72%,表現(xiàn)為良好的準確度和精密度。
[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.

【學位授予單位】：浙江海洋大學
【學位級別】：碩士
【學位授予年份】：2017
【分類號】：O657.63;TS218

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本文編號：1439178