豬肉中典型重金屬元素的雙脈沖激光誘導(dǎo)擊穿光譜檢測研究
發(fā)布時間：2019-03-12 20:02
【摘要】：我國是世界豬肉生產(chǎn)和消費第一大國,而生豬在養(yǎng)殖、屠宰、流通過程都有被重金屬污染的可能,豬肉重金屬殘留量也是食品衛(wèi)生安全要求的必檢項目。傳統(tǒng)化學(xué)分析方法的前處理繁瑣且會對環(huán)境造成污染,因此需要探索綠色檢測方法。激光誘導(dǎo)擊穿光譜(Laser induced breakdown spectroscopy,LIBS)是一種具有綠色、快速、原位檢測特點的發(fā)射光譜檢測技術(shù),可以滿足綠色在線檢測需求。本工作利用雙脈沖激光誘導(dǎo)擊穿光譜(Dual-pulse laser induced breakdown spectroscopy,DP-LIBS)對豬肉中典型重金屬元素鎘(Cd)、鉛(Pb)和鉻(Cr)進行快速綠色檢測研究,進一步結(jié)合微波輔助雙脈沖LIBS(Microwave assisted dual-pulse laser induced breakdown spectroscopy,MA-DP-LIBS)檢測豬肉標(biāo)準(zhǔn)物質(zhì)樣品中的重金屬元素Cd和Pb,探究微波對LIBS光譜中Cd和Pb的增強效果。論文主要研究內(nèi)容如下:以豬肉樣品中典型重金屬元素Cd、Pb、Cr為研究對象,結(jié)合LIBS光譜數(shù)據(jù)與目標(biāo)元素濃度進行定量分析。對試驗樣品進行DP-LIBS測試后,分別采用陽極溶出伏安法(Anodic stripping voltammetry,ASV)和原子吸收光譜法(Atomic absorption spectrometry,AAS)檢測得到樣品中Cd和Pb、Cr濃度。將Cd、Pb強度值與濃度值進行單變量線性擬合,擬合系數(shù)分別為0.90、0.55。在標(biāo)準(zhǔn)正態(tài)變量變換(Standard normal variable transformation,SNV)、一階導(dǎo)數(shù)(First derivative,FD)、二階導(dǎo)數(shù)(Second derivative,SD)、多元散射校正(Multiple scattering correction,MSC)和均值中心化(Mean centralized,MC)五種預(yù)處理方法中選擇最佳預(yù)處理方法MC,分別進行偏最小二乘(Partial least squares,PLS)、間隔偏最小二乘(Interval partial least squares,iPLS)和聯(lián)合間隔偏最小二乘(Synergy interval partial least squares,Si PLS)建模,以交叉驗證均方根誤差(RMSECV)、預(yù)測均方根誤差(RMSEP)、對應(yīng)的訓(xùn)練相關(guān)系數(shù)(RC)、預(yù)測相關(guān)系數(shù)(RP)為檢驗標(biāo)準(zhǔn)對LIBS光譜數(shù)據(jù)進行分析比較。結(jié)果顯示,三種元素的擬合系數(shù)均達到0.95以上,Cd擬合最佳效果高達0.9986。結(jié)論表明,PLS、i PLS和SiPLS模型均可對豬肉中Cd、Pb、Cr進行分析,這為豬肉中重金屬元素LIBS檢測提供了參考依據(jù)。結(jié)合MA-DP-LIBS對豬肉標(biāo)準(zhǔn)物質(zhì)樣品中重金屬元素Cd、Pb進行檢測研究。結(jié)果顯示,采用豬肉標(biāo)準(zhǔn)物質(zhì)代替原始豬肉可使Cd、Pb的干樣濃度最低檢出限由11.10mg/kg、8.58 mg/kg降低為9 mg/kg、4 mg/kg,且MA-DP-LIBS對大部分元素增強效果顯著,而Cd在MA-DP-LIBS測試下會受到其它基質(zhì)元素干擾導(dǎo)致譜線被覆蓋。結(jié)論表明,MA-DP-LIBS對豬肉標(biāo)準(zhǔn)物質(zhì)中Pb元素有信號增強效果。
[Abstract]:China is the world's largest country in pork production and consumption, and pig breeding, slaughtering, circulation process are likely to be contaminated by heavy metals, pork heavy metal residue is also a food hygiene and safety requirements of the necessary inspection items. The pretreatment of traditional chemical analysis methods is cumbersome and will pollute the environment, so it is necessary to explore green detection methods. Laser-induced breakdown spectroscopy (Laser induced breakdown spectroscopy,LIBS) is a green, fast, in-situ emission spectrum detection technique, which can meet the needs of green on-line detection. In this work, double pulse laser induced breakdown spectroscopy (Dual-pulse laser induced breakdown spectroscopy,DP-LIBS) was used to detect the typical heavy metal elements CD, (Cd), Pb, (Pb) and Cr-(Cr) in pork. The enhancement of Cd and Pb in LIBS spectra by microwave assisted double pulse LIBS (Microwave assisted dual-pulse laser induced breakdown spectroscopy,MA-DP-LIBS (microwave assisted double pulse Cd) detection of heavy metal elements (Cd and Pb,) in pork reference material samples was investigated. The main contents of this paper are as follows: taking the typical heavy metal element Cd,Pb,Cr in pork samples as the research object, the quantitative analysis was carried out by combining the LIBS spectral data with the concentration of the target elements. After DP-LIBS, the concentrations of Cd and Pb,Cr in the samples were determined by anodic stripping voltammetry (Anodic stripping voltammetry,ASV) and atomic absorption spectrometry (Atomic absorption spectrometry,AAS), respectively. The linear fitting coefficients of Cd,Pb intensity and concentration were 0.90,0.55 respectively. In standard normal variable transformation (Standard normal variable transformation,SNV), first derivative (First derivative,FD), second derivative (Second derivative,SD), multivariate scattering correction (Multiple scattering correction,MSC and mean centralization (Mean centralized, Among the five pretreatment methods, MC, (partial least Squares (Partial least squares,PLS), interval partial least Squares (Interval partial least squares,iPLS) and Joint interval partial least Squares (Synergy interval partial least squares,Si PLS) are selected to model MC). The training correlation coefficient (RC),) prediction correlation coefficient (RP) corresponding to the root mean square error (RMSEP),) prediction of root mean square error (RMSECV),) was used as the test standard to analyze and compare the LIBS spectral data. The results showed that the fitting coefficients of the three elements were above 0.95, and the best fitting effect of Cd was 0.9986. The results show that both PLS,i PLS and SiPLS models can be used to analyze the Cd,Pb,Cr in pork, which provides a reference for the detection of heavy metal element LIBS in pork. The determination of heavy metal element (Cd,Pb) in pork reference material samples by MA-DP-LIBS was studied. The results showed that the detection limit of Cd,Pb could be reduced from 11.10 mg / kg to 9 mg/kg,4 mg/kg, by using pork reference material instead of raw pork. Moreover, the enhancement effect of MA-DP-LIBS on most of the elements is remarkable, while the Cd will be interfered by other matrix elements under the MA-DP-LIBS test, and the spectral lines will be covered. The results showed that MA-DP-LIBS could enhance the signal of Pb in pork reference material.
【學(xué)位授予單位】：江西農(nóng)業(yè)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TS251.51;O657.3
本文編號：2439106
[Abstract]:China is the world's largest country in pork production and consumption, and pig breeding, slaughtering, circulation process are likely to be contaminated by heavy metals, pork heavy metal residue is also a food hygiene and safety requirements of the necessary inspection items. The pretreatment of traditional chemical analysis methods is cumbersome and will pollute the environment, so it is necessary to explore green detection methods. Laser-induced breakdown spectroscopy (Laser induced breakdown spectroscopy,LIBS) is a green, fast, in-situ emission spectrum detection technique, which can meet the needs of green on-line detection. In this work, double pulse laser induced breakdown spectroscopy (Dual-pulse laser induced breakdown spectroscopy,DP-LIBS) was used to detect the typical heavy metal elements CD, (Cd), Pb, (Pb) and Cr-(Cr) in pork. The enhancement of Cd and Pb in LIBS spectra by microwave assisted double pulse LIBS (Microwave assisted dual-pulse laser induced breakdown spectroscopy,MA-DP-LIBS (microwave assisted double pulse Cd) detection of heavy metal elements (Cd and Pb,) in pork reference material samples was investigated. The main contents of this paper are as follows: taking the typical heavy metal element Cd,Pb,Cr in pork samples as the research object, the quantitative analysis was carried out by combining the LIBS spectral data with the concentration of the target elements. After DP-LIBS, the concentrations of Cd and Pb,Cr in the samples were determined by anodic stripping voltammetry (Anodic stripping voltammetry,ASV) and atomic absorption spectrometry (Atomic absorption spectrometry,AAS), respectively. The linear fitting coefficients of Cd,Pb intensity and concentration were 0.90,0.55 respectively. In standard normal variable transformation (Standard normal variable transformation,SNV), first derivative (First derivative,FD), second derivative (Second derivative,SD), multivariate scattering correction (Multiple scattering correction,MSC and mean centralization (Mean centralized, Among the five pretreatment methods, MC, (partial least Squares (Partial least squares,PLS), interval partial least Squares (Interval partial least squares,iPLS) and Joint interval partial least Squares (Synergy interval partial least squares,Si PLS) are selected to model MC). The training correlation coefficient (RC),) prediction correlation coefficient (RP) corresponding to the root mean square error (RMSEP),) prediction of root mean square error (RMSECV),) was used as the test standard to analyze and compare the LIBS spectral data. The results showed that the fitting coefficients of the three elements were above 0.95, and the best fitting effect of Cd was 0.9986. The results show that both PLS,i PLS and SiPLS models can be used to analyze the Cd,Pb,Cr in pork, which provides a reference for the detection of heavy metal element LIBS in pork. The determination of heavy metal element (Cd,Pb) in pork reference material samples by MA-DP-LIBS was studied. The results showed that the detection limit of Cd,Pb could be reduced from 11.10 mg / kg to 9 mg/kg,4 mg/kg, by using pork reference material instead of raw pork. Moreover, the enhancement effect of MA-DP-LIBS on most of the elements is remarkable, while the Cd will be interfered by other matrix elements under the MA-DP-LIBS test, and the spectral lines will be covered. The results showed that MA-DP-LIBS could enhance the signal of Pb in pork reference material.
【學(xué)位授予單位】：江西農(nóng)業(yè)大學(xué)
【學(xué)位級別】：碩士
【學(xué)位授予年份】：2017
【分類號】：TS251.51;O657.3
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