CN102928377B - 一种明胶及其制品中六价铬的测定方法 - Google Patents

一种明胶及其制品中六价铬的测定方法 Download PDF

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CN102928377B
CN102928377B CN201210388880.5A CN201210388880A CN102928377B CN 102928377 B CN102928377 B CN 102928377B CN 201210388880 A CN201210388880 A CN 201210388880A CN 102928377 B CN102928377 B CN 102928377B
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宋薇
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PONY TESTING INTERNATIONAL GROUP SHANGHAI CO., LTD.
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Abstract

本发明公开了一种明胶及其制品中六价铬的测定方法。包括下列步骤：试样中加入MgCl2、磷酸盐缓冲液和Na2CO3/NaOH溶液，置于75-85℃水浴振荡消解0.5-1.5h；冷却至室温，用0.45μm滤膜抽滤；取滤液于电热板上进行酸消解；消解液稀释、定容后，用原子吸收分光光度法测定六价铬含量。本方法采用酸消解除去基质干扰，专属性强、灵敏度高、结果准确。

Description

一种明胶及其制品中六价铬的测定方法
技术领域
本发明涉及一种六价铬的测定方法，特别是涉及一种明胶及其制品中六价铬的测定方法。
背景技术
铬的毒性与其存在的价态有关。六价铬，是一种强致癌物质，比三价铬毒性高100倍，而且易被人体吸收并在体内蓄积，对人的生存环境和身体健康有着显著的危害。由于市场上发现某些不法明胶生产厂家违法使用皮革下脚料“蓝矾皮”作为原料生产的工业明胶，冒充食用明胶或药用明胶。工业明胶常含有高含量的铬，其中会含有毒性大的六价铬，引起社会的密切关注。
六价铬的测定方法有很多，如：分光光度法、离子色谱法、原子吸收光谱法、毛细管电泳、荧光分析法、化学发光法、电化学分析法等。上述方法常用于来自于制革、冶矿冶金、电镀、印染行业等样品中六价铬的测定，文献中未发现有测定明胶及其制品中六价铬的方法。SN/T2210-2008保健食品中六价铬的测定离子色谱-电感耦合等离子体质谱法采用Na2CO3/NaOH溶液同时加入MgCl2和磷酸盐缓冲液提取六价铬，提取液离心后，直接用离子色谱-电感耦合等离子体质谱测定。方法所用仪器属联用技术且电感耦合等离子体质谱仪比较昂贵，一般实验室难以普及。EPA3060A六价铬碱式消解，采用Na2CO3/NaOH溶液同时加入MgCl2和磷酸盐缓冲液提取六价铬，提取液调节pH后，采用紫外分光光度法或离子色谱法测定，方法适用于受污土壤或污泥等废弃物。本发明针对明胶及其制品，碱式消解后，明胶中的蛋白未被消解，有机物质干扰严重，容易堵塞原子吸收光谱仪燃烧器的管路。
发明内容
本发明一种明胶及其制品中六价铬的测定方法，包括以下步骤：
1.实验操作
称取试样2.0-5.0g于250mL的玻璃三角瓶中，加入400mgMgCl2、0.5mLpH＝7磷酸盐缓冲液，加入消解溶液(0.28MNa2CO3/0.5MNaOH)25或50mL。用微波保鲜膜封口，置于75-85℃水浴振荡消解0.5-1.5h。消解完毕，冷却至室温，用0.45μm滤膜抽滤，取10mL滤液于50mL小烧杯中，加入10mL无机酸(无机酸为硝酸、盐酸、高氯酸、或其混合酸，优选硝酸)，盖上表面皿于电热板上酸消解。消解至澄清后，浓缩至2mL左右，冷却至室温，转移至10mL容量瓶中，并用蒸馏水定容，摇匀，待测。
2.光谱测定
Cr(VI)标准储备液：准确称取0.2829g在105℃-110℃烘干的重铬酸钾标准品，用蒸馏水溶解并稀释至100mL，此溶液Cr(VI)浓度为1mg/mL。
Cr(VI)标准工作液：取5mL铬(VI)标准储备液，用蒸馏水稀释至100mL，此溶液Cr(VI)浓度为50μg/mL。
取上述工作液，然后进一步用水稀释为具有浓度梯度的标准使用液；
利用原子吸收分光光度仪对试样进行检测，外标法定量。
本发明的技术效果在于：
①建立了原子吸收分光光度法检测明胶及其制品中的六价铬的方法。该方法仪器较普遍、干扰小、专属性强、成本低、易普及推广。
②前处理方法简单有效。采用碱性消解液提取明胶及其制品，在碱性环境中Cr(III)和Cr(VI)氧化还原性都被降到最低，含有MgCl2的磷酸盐缓冲溶液可以抑制铬的氧化作用，在此碱性环境下三价铬被提取出来会以沉淀的形式被过滤除去，从而排除三价铬的干扰。
③该方法合理可行，结果准确。碱消解除去三价铬后再采用酸消解样品中的有机物，去除基质干扰，具有较好的净化效果，上机检测灵敏度高。
具体实施方式
下面结合具体实施例对本发明作进一步详细说明，但本发明并不局限于具体实施例。
实施例1
1.1样品测定
精确称取某红色明胶空心胶囊5.00g于250mL的玻璃三角瓶中，加入400mgMgCl2、0.5mL磷酸盐缓冲液，加入消解溶液至50mL。用微波保鲜膜封口，置于80℃水浴振荡消解1h。消解完毕，冷却至室温，用0.45μm滤膜抽滤，取10mL滤液置于50mL小烧杯中，加入10mL硝酸，盖上表面皿于电热板上酸消解。消解至澄清后，浓缩至2mL左右，冷却至室温，转移至10mL容量瓶中，并用蒸馏水定容，摇匀，待测。
1.2原子吸收分光光度法测定
按照光谱条件测定样品和标准工作溶液，用标准曲线对样品溶液浓度进行校正，外标法定量。光谱条件为：
原子吸收分光光度计(火焰法)，铬空心阴极灯；
测定波长：357.9nm；
狭缝宽度：0.2nm；
灯电流：3.00mA
1.3线性关系
将标准工作液用12％硝酸逐级稀释，制备0.1，0.2，0.5，1.0，2.0，5.0μg/mL不同浓度的系列混合标准溶液，按照上述光谱条件由低到高浓度顺序测定标准溶液的吸光度。用吸光度与相对应的铬的浓度(μg/mL)绘制标准曲线，回归方程为Y＝0.0585X+0.0055，相关系数为0.9998。
1.4空白试验
在不加试样条件下，其它步骤均同1.1，在测试样品同时进行空白试验。
1.5实际样品加标回收率
采用上述红色明胶空心胶囊阴性样品进行加标测定其回收率，加标量分别为25μg和100μg，每个浓度测定3个平行样品，按照步骤(1.1)进行提取、测定。平均回收率分别为85.6％和95.7％，相对标准偏差分别为5.7％和10.0％。
实施例2
按照实施例1所述的实验步骤，对某明胶阴性样品进行加标测定三价铬对六价铬的影响。分别称取样品5.0g各6份，其中三份添加Cr(VI)100μg，另外三份添加Cr(VI)和Cr(III)各100μg，按照步骤1.1进行提取、测定。只添加Cr(VI)的样品的平均回收率为94.6％，添加Cr(VI)和Cr(III)的样品的平均回收率为92.6％，相对标准偏差分别为9.9％和9.8％。两者回收率和相对标准偏差相差都很小。因此，三价铬对六价铬的回收率没有明显影响。
上述实施例仅供说明本发明之用，而并非是对本发明的限制，有关技术领域的普通技术人员，在不脱离本发明范围的情况下，还可以作出各种变化和变型，因此所有等同的技术方案也应属于本发明的范畴，本发明的专利保护范围应由各权利要求限定。

Claims (2)

1.一种明胶及其制品中六价铬的测定方法，包括下列步骤：
(1)试样加入Na2CO3/NaOH溶液，同时加入MgCl2和磷酸盐缓冲液，水浴振荡消解；
(2)碱消解完毕，冷却后用滤膜抽滤除去三价铬沉淀；
(3)取滤液加无机酸于电热板上进行湿法酸消解；
(4)消解液用蒸馏水稀释、定容，用原子吸收分光光度法测定六价铬含量。
2.根据权利要求1所述的一种明胶及其制品中六价铬的测定方法，其特征在于，所述的水浴振荡温度为75-85℃。
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