CN108254344A - 一种利用结晶紫测定三聚氰胺的方法 - Google Patents

一种利用结晶紫测定三聚氰胺的方法 Download PDF

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CN108254344A
CN108254344A CN201810004487.9A CN201810004487A CN108254344A CN 108254344 A CN108254344 A CN 108254344A CN 201810004487 A CN201810004487 A CN 201810004487A CN 108254344 A CN108254344 A CN 108254344A
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melamine
solution
light intensity
scattered light
crystal violet
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CN108254344B (zh
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唐宁莉
范晶晶
马小龙
王文平
黄文琪
张容珲
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Guilin University of Technology
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    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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    • G01N21/6428—Measuring fluorescence of fluorescent products of reactions or of fluorochrome labelled reactive substances, e.g. measuring quenching effects, using measuring "optrodes"
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    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G—PHYSICS
    • G01—MEASURING; TESTING
    • G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/62—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light
    • G01N21/63—Systems in which the material investigated is excited whereby it emits light or causes a change in wavelength of the incident light optically excited
    • G01N21/64—Fluorescence; Phosphorescence
    • G01N2021/6417—Spectrofluorimetric devices

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Abstract

本发明公开了一种利用结晶紫测定三聚氰胺的方法。8支10mL比色管中依次加入0.1、0.5、1.0、2.0、3.0、4.0、5.0、6.0 mL 1000μg/L的三聚氰胺溶液，再分别加入伯瑞坦‑罗宾森缓冲溶液、结晶紫溶液，以不加三聚氰胺的溶液为试剂空白，定容至刻度，反应后，于荧光光度计上，用1cm比色皿，设置λem=λex=394nm，狭缝5 nm，电压600V，分别测定含三聚氰胺溶液的散射强度I和试剂空白的散射强度I 0 ，计算散射强度差值Δ I=I‑I 0 。在纯牛奶中加入三氯乙酸和乙酸铅溶液，超声，离心，依上述方法测定散射强度值，计算出牛奶中三聚氰胺的含量。本发明方法灵敏度高、操作简便快捷。

Description

一种利用结晶紫测定三聚氰胺的方法
技术领域
本发明涉及三聚氰胺的测定方法，特别是利用结晶紫采用共振散射技术测定三聚氰胺的方法。
背景技术
三聚氰胺(Melamine，MEL)是重要的氮杂环有机化工原料，主要用于制作三聚氰胺-甲醛树脂，也广泛应用于纺织助剂、皮革柔润剂、上光剂、抗水剂、黏合剂等的生产中。在鲜奶及乳制品中添加三聚氰胺，可显著提高含氮量，用以冒充高蛋白食品，从而大幅度降低成本。自2008年爆发毒奶粉事件后，食品中三聚氰胺的快速检测成为了人们亟需解决的问题。三聚氰胺的含量测定多采用色谱法，虽然检测精度高，但分析成本高昂，耗时较长；此外还有化学发光法、电化学法、分光光度法、荧光法和共振散射光谱法等。其中共振散射光谱法是一种高灵敏度、快速、简便的分析方法，可用于痕量无机物和有机物的分析。结晶紫(Crystal Violet，CV)是一种三苯甲烷系碱性染料，常用于金属离子的测定，但利用结晶紫与三聚氰胺反应，采用共振散射光谱法检测三聚氰胺的含量尚未见文献报道。
发明内容
本发明的目的是提供一种结晶紫共振散射法测定三聚氰胺的方法。
具体步骤为：
(1)于8支10mL比色管中依次加入0.1、0.5、1.0、2.0、3.0、4.0、5.0、6.0mL 1000μg/L的三聚氰胺溶液，再在每支管中分别加入1.0mL pH2.4的伯瑞坦-罗宾森(Britton-Robinson)缓冲溶液、1.0mL浓度为4.0×10-5mol/L的结晶紫溶液，以不加三聚氰胺的溶液为试剂空白，然后用超纯水将8支比色管定容至刻度，在25℃的水浴中反应10分钟后，于荧光光度计上，用1cm比色皿，设置
λem＝λex＝394nm，狭缝5nm，电压600V，分别测定含三聚氰胺溶液的散射光强度I和试剂空白的散射光强度I0，计算散射光强度差值ΔI＝I-I0，其散射光强度差值ΔI与三聚氰胺质量浓度ρ在10～600μg/L范围内成线性关系，线性回归方程为：ΔI＝0.5751ρ-3.936(ρ的单位为μg/L)，相关系数0.9989，检出限为1.33μg/L。
(2)取市售纯牛奶10.0mL，加入5.0mL质量百分比浓度为1％的三氯乙酸和5.0mL质量百分比浓度为2％的乙酸铅溶液，超声20分钟。然后取部分溶液于离心管中，离心10分钟，取上清液作为待测液。
(3)取步骤(2)处理后的牛奶待测液0.1mL，依步骤(1)的方法测定散射光强度值，计算出牛奶中三聚氰胺的含量。
本发明方法灵敏度高、操作简便快捷。
附图说明
附图为本发明实施例空白与400μg/L三聚氰胺的共振散射光谱图。
图中标记：a：空白；b：空白-400μg/L MEL。
具体实施方式
实施例：
(1)于8支10mL比色管中依次加入0.1、0.5、1.0、2.0、3.0、4.0、5.0、6.0mL浓度为1000μg/L的三聚氰胺溶液，再在每支比色管中分别加入1.0mL pH2.4的伯瑞坦-罗宾森(Britton-Robinson，B-R)缓冲溶液、1.0mL浓度为4.0×10-5mol/L的结晶紫溶液，以不加三聚氰胺的溶液为试剂空白，然后用超纯水将8支比色管定容至刻度，在25℃的水浴中反应10分钟后，于荧光光度计上，用1cm比色皿，设置λem＝λex＝394nm，狭缝5nm，电压600V，分别测定含三聚氰胺溶液的散射光强度I和试剂空白的散射光强度I0，计算散射光强度差值ΔI＝I-I0，其散射光强度差值ΔI与三聚氰胺质量浓度ρ在10～600μg/L范围内成线性关系，线性回归方程为：ΔI＝0.5751ρ-3.936(ρ的单位为μg/L)，相关系数0.9989，检出限为1.33μg/L。
(2)取10.0mL市售蒙牛纯牛奶，加入5.0mL质量百分比浓度为1％的三氯乙酸和5.0mL质量百分比浓度为2％的乙酸铅溶液，超声20分钟。然后取部分溶液于离心管中，离心10分钟，取上清液作为待测液。
(3)取0.1mL步骤(2)处理后的牛奶待测液，依步骤(1)的方法测定散射光强度值，计算出牛奶中三聚氰胺的含量。同时做了加标回收实验，结果见表1。
表1：蒙牛纯牛奶三聚氰胺测定结果(n＝5)

Claims (1)

1.一种利用结晶紫测定三聚氰胺的方法，其特征在于具体步骤为：
（1）于8支10mL比色管中依次加入0.1、0.5、1.0、2.0、3.0、4.0、5.0、6.0 mL浓度为1000μg/L的三聚氰胺溶液，再在每支管中分别加入1.0mL pH2.4的伯瑞坦-罗宾森缓冲溶液、1.0mL浓度为4.0×10-5mol/L的结晶紫溶液，以不加三聚氰胺的溶液为试剂空白，然后用超纯水将8支比色管定容至刻度，在25℃的水浴中反应10分钟后，于荧光光度计上，用1cm比色皿，设置λem=λex=394nm，狭缝5 nm，电压600V，分别测定含三聚氰胺溶液的散射光强度I和试剂空白的散射光强度I 0 ，计算散射光强度差值ΔI=I-I 0 ，其散射光强度差值ΔI与三聚氰胺质量浓度ρ在10～600μg/L范围内成线性关系，线性回归方程为：ΔI=0.5751ρ-3.936,ρ的单位为μg/L），相关系数0.9989，检出限为1.33μg/L；
（2）取10.0mL市售纯牛奶，加入5.0mL质量百分比浓度为1%的三氯乙酸和5.0mL质量百分比浓度为2%的乙酸铅溶液，超声20分钟；然后取部分溶液于离心管中，离心10分钟，取上清液作为待测液；
（3）取0.1mL步骤（2）处理后的牛奶待测液，依步骤（1）的方法测定散射光强度值，计算出牛奶中三聚氰胺的含量。
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