CN109115764A - 环保型尿液羟苯衍生物检测试剂及其制备方法 - Google Patents

环保型尿液羟苯衍生物检测试剂及其制备方法 Download PDF

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CN109115764A
CN109115764A CN201810851159.2A CN201810851159A CN109115764A CN 109115764 A CN109115764 A CN 109115764A CN 201810851159 A CN201810851159 A CN 201810851159A CN 109115764 A CN109115764 A CN 109115764A
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邓兴朝
黄连生
穆洪涛
李嘉慧
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Abstract

本发明公开了一种环保型尿液羟苯衍生物检测试剂的制备方法,包括以下步骤:称取汞溶于浓硝酸中,再加入约2倍浓硝酸体积的超纯水,得到A溶液;称取硝酸亚汞溶于浓硝酸中,得到B溶液;称取对二甲氨基苯甲醛溶于硫酸中,得到C溶液;称取硝酸镍溶于超纯水中,得到D溶液;取WS2纳米材料用硝酸处理,得到E溶液;将制备的A、B、C、D、E溶液按1:0.2~0.55:0.14~0.2:0.07~0.08:0.01比例混合,摇匀,即得该尿液羟苯衍生物检测试剂。本发明制备的环保型尿液羟苯衍生物检测试剂使用便捷,检测时间短,对肿瘤的检出率高于现有的检测试剂,且该检测试剂对环境友好。

Description

环保型尿液羟苯衍生物检测试剂及其制备方法
技术领域
本发明涉及尿液检测试剂领域,具体涉及一种环保型尿液羟苯衍生物检测试剂及其制备方法。
背景技术
当今社会,癌症成为严重威胁人类健康的全球问题。研究证实,当人体有肿瘤细胞活动时,细胞的异常增殖引发应激反应引起人体羟苯衍生物(酪氨酸、色氨酸、儿茶酚胺、香草扁桃酸(VMA)、高香草酸(HVA)、对羟苯丙酮酸、5-羟吲哚乙酸、2,5-羟苯乙酸、多巴胺、5-羟色胺等)的分泌增加,并且这类物质可以通过尿液排放。
目前市场上已有的显色试剂主要以重金属离子Hg2+与羟苯衍生物的巯基结合形成红色特征物,但并未对其成分中存在对环境具有污染性的重金属离子(如:Hg2+、Hg2 2+、Ni2+)进行处理(如专利号:CN 102565055、CN 104535565)。这些未进行科学处理的废弃液会加重环境的负担,导致水资源和土壤的重金属污染。
发明内容
本发明的目的是为了提供一种环保型尿液羟苯衍生物检测试剂及其制备方法,旨在提供一种检测效率高,对环境友好的尿液羟苯衍生物检测试剂。
为此,本发明所采用的技术方案为:
一种环保型尿液羟苯衍生物检测试剂的制备方法,其中,包括以下步骤:
称取汞溶于浓硝酸中,再加入约2倍浓硝酸体积的超纯水,得到A溶液;
称取硝酸亚汞溶于浓硝酸中,得到B溶液;
称取对二甲氨基苯甲醛溶于硫酸中,得到C溶液;
称取硝酸镍溶于超纯水中,得到D溶液;
取WS2纳米材料用硝酸处理,得到E溶液;
将制备的A、B、C、D、E溶液按1:0.2~0.55:0.14~0.2:0.07~0.08:0.01比例混合,摇匀,即得该尿液羟苯衍生物检测试剂。
所述的环保型尿液羟苯衍生物检测试剂的制备方法,其中,制备B溶液所用的浓硝酸摩尔浓度为4.5moL/L。
所述的环保型尿液羟苯衍生物检测试剂的制备方法,其中,所述B溶液为硝酸亚汞溶液,其浓度为210~245g/L。
所述的环保型尿液羟苯衍生物检测试剂的制备方法,其中,制备C溶液所用的硫酸的摩尔浓度为10.7moL/L。
所述的环保型尿液羟苯衍生物检测试剂的制备方法,其中,所述C溶液为二甲氨基苯甲醛溶液,其浓度为3~5g/L。
所述的环保型尿液羟苯衍生物检测试剂的制备方法,其中,所述D溶液为硝酸镍溶液,其浓度为300~500g/L。
所述的环保型尿液羟苯衍生物检测试剂的制备方法,其中,制备E溶液所用的硝酸摩尔浓度为6mol/L。
所述的环保型尿液羟苯衍生物检测试剂的制备方法,其中,所述E溶液为纳米胶体溶液,其浓度为0.3~0.7g/L。
所述的环保型尿液羟苯衍生物检测试剂的制备方法,其中,WS2纳米材料的X射线衍射结果为六边形2H-WS2,粒径为1μm。
一种环保型尿液羟苯衍生物检测试剂,其中,采用如权利要求1-9任一项所述的方法制备得到。
有益效果:本发明提供一种环保型尿液羟苯衍生物检测试剂及其制备方法,该检测试剂使用便捷,检测时间短,对肿瘤的检出率高于现有的检测试剂,且该检测试剂对环境友好。
具体实施方式
下面通过实施例进一步阐述本发明的技术方案,但本发明要求保护的范围并不局限于实施例表示的范围。
本发明提供一种环保型尿液羟苯衍生物检测试剂的制备方法,其中,包括以下步骤:
A溶液的制备:称取汞溶于浓硝酸中,再加入约2倍浓硝酸体积的超纯水,得到A溶液。
B溶液的制备:称取硝酸亚汞溶于4.5moL/L浓硝酸中,得到210~245g/L的硝酸亚汞溶液。
C溶液的制备:称取对二甲氨基苯甲醛溶于10.7moL/L的硫酸中,得到3~5g/L的对二甲氨基苯甲醛溶液。
D溶液的制备:称取硝酸镍溶于超纯水中,得到300~500g/L的硝酸镍溶液。
E溶液的制备:取WS2纳米材料,用6mol/L的硝酸处理,得到0.3~0.7g/L的纳米胶体溶液。
混合:将制备的A、B、C、D、E溶液按1:0.2~0.55:0.14~0.2:0.07~0.08:0.01比例混合,摇匀,即得该尿液羟苯衍生物检测试剂。
具体的,该尿液羟苯衍生物检测试剂具有良好的稳定性,其可在密封条件下保存1年。
本发明的制备方法所得的尿液羟苯衍生物检测试剂,使用方法:
(1)被检者尿液采样:取早晨第一次尿液的中段部分,用滴管吸取3mL尿液加入到装有0.6±0.1mL显色试剂的显色瓶中,摇匀后静置。待2~4min显色稳定后,观察尿液沉淀颜色。
(2)显色结果:若尿液沉淀为白色或黄色,则检测结果为阴性,若尿液沉淀为浅紫色或浅红色,则检测结果为弱阳性,若尿液沉淀为紫红色,则检测结果为阳性。检测结果为阳性时,需在排除药物干扰一周后另作一次检测,若检测结果相同,建议及时到医院接受检查和治疗。
(3)以上检测效果在被检者检测前三日内停止服用氨基酸类、激素类药品,镇静类、止痛类、降压类药物,神经系统兴奋剂,抗菌素,保健品以及高蛋白食物等情况下为佳。
(4)WS2纳米花材料作为检测试剂的载体,此材料XRD结果显示结构为六边形2H-WS2,粒径为1μm,具有很高比表面积。通过静电作用吸附重金属离子Hg2+,从而达到增加显色速率、显色均一稳定、废弃物处理环保的效果。
经临床试验,本发明的制备方法所得的尿液羟苯衍生物检测试剂,对肿瘤检出率高达95.6%,并且能更好地处理废弃物,环境友好。
显色速率对比:
选取ABCD液与硝酸的混合液α液与ABCDE的混合液β液各0.6mL与相同尿液样品3mL置于4℃、15℃、25℃的环境下进行显色反应。反应所用时长如下:
α液 β液
4℃ 10min 3.5min
15℃ 5min 2.5min
25℃ 3.0min 2.1min
重金属吸附对比:
1组:取ABCD液与硝酸的混合液0.6mL加入3mL尿液混匀,经湿法消化,定容到100mL,用火焰原子吸收光谱法测定其中的Hg、Ni含量,浓度分别为0.77±0.02g/L、0.03±0.005g/L。
2组:取ABCDE液的混合液0.6mL加入3mL尿液混匀,经湿法消化后,消化液定容到100mL,用火焰原子吸收光谱法测定其中的Hg、Ni含量,浓度分别为2.3×10-3g/L、9×10-5g/L,去除效率均达到99.7%。
下面通过实施例进一步说明本发明技术方案。
实施例1
配制1100mL的尿液羟苯衍生物检测试剂
A溶液的制备:称取120g汞溶于180mL浓硝酸中,再加入2倍浓硝酸体积的超纯水,得到A溶液。
B溶液的制备:称取70g硝酸亚汞溶于适量的4.5moL/L的浓硝酸中,得到241g/L的硝酸亚汞溶液。
C溶液的制备:称取4.15g对二甲氨基苯甲醛溶于950mL10.7moL/L硫酸中,再用蒸馏水定容至1000mL,得到4.15g/L的对二甲氨基苯甲醛溶液。
D溶液的制备:称取50g硝酸镍溶于100mL超纯水中,得到500g/L的硝酸镍溶液。
E溶液的制备:取0.11gWS2纳米花,用200mL6mol/L的硝酸处理,得到0.55g/L的纳米胶体溶液。
混合:将制备的A、B、C、D、E溶液按1:0.4:0.16:0.6:0.07:0.01比例混合,摇匀即配成1100mL本试剂。
实施例2
配制1100mL的尿液羟苯衍生物检测试剂
A溶液的制备:称取90g汞溶于180mL浓硝酸中,再加入2倍浓硝酸体积的超纯水,得到A溶液。
B溶液的制备:称取450g硝酸亚汞溶于适量的4moL/L的浓硝酸中,得到150g/L的硝酸亚汞溶液。
C溶液的制备:称取4.15g对二甲氨基苯甲醛溶于950mL10.7moL/L硫酸中,再用蒸馏水定容至1000mL,得到4.15g/L的对二甲氨基苯甲醛溶液。
D溶液的制备:称取400g硝酸镍溶于适量超纯水中,得到200g/L的硝酸镍溶液。
E溶液的制备:取0.11gWS2纳米花,用200mL 6mol/L的硝酸处理,得到0.55g/L纳米胶体溶液。
将制备的A、B、C、D溶液按1:0.7:0.3:0.7:0.05比例混合,摇匀即配成1100mL本试剂。
实施例3
临床试验结果
1.试验对象
肿瘤组:经临床诊断确诊的肿瘤患者210名,根据其肿瘤的发生部位分为胃、肝、结肠、食管、肺、前列腺、膀胱、子宫颈、乳腺、淋巴组。
对照组:经检查健康合格的正常健康人47名。
试验要求被检者在检查前三日内停止服药及保健品和相关食品,具体包括氨基酸类、激素类药品,镇静类、止痛类、降压类药物,神经系统兴奋剂,抗菌素,保健品以及高蛋白食物等。
2.试验方法
取被检者早晨第一次尿液的中段部分,分别用滴管吸取3mL尿液加入到实施例1和实施例3所配制的显色液中,摇匀后静置。待2~4min显色稳定后,观察尿液沉淀颜色。其中47个正常人尿液样品由经检查健康合格者提供。
3.试验结果
表1为采用实施例1显色试剂检测各组尿液结果
肿瘤类别 人数 阳性人数 阴性人数 准确率
28 28 0 100.00%
22 21 1 95.45%
结肠 18 18 0 100.00%
食管 26 25 1 96.15%
13 9 4 69.23%
前列腺 31 27 4 87.10%
膀胱 17 17 0 100.00%
子宫颈 25 24 1 96.00%
乳腺 22 21 1 95.45%
淋巴 8 6 2 75.00%
正常人 47 1 46 97.87%
表2为采用实施例2显色试剂检测各组尿液结果
如上表所示,实施例1制备的尿液羟苯衍生物检测试剂对上述恶性肿瘤的检出率均超过95%。实施例2制备的显色试剂对肿瘤的检出率较实施例1制备的显色试剂低。由此可见,本发明的尿液羟苯衍生物检测试剂对肿瘤的检出率高于现有的检测试剂。与原有试剂相比,检测结果更精确。
综上所述,本发明制备的环保型尿液羟苯衍生物检测试剂使用便捷,检测时间短,对肿瘤的检出率高于现有的检测试剂,且该检测试剂对环境友好。
应当理解的是,本发明的应用不限于上述的举例,对本领域普通技术人员来说,可以根据上述说明加以改进或变换,所有这些改进和变换都应属于本发明所附权利要求的保护范围。

Claims (10)

1.一种环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,包括以下步骤:
称取汞溶于浓硝酸中,再加入约2倍浓硝酸体积的超纯水,得到A溶液;
称取硝酸亚汞溶于浓硝酸中,得到B溶液;
称取对二甲氨基苯甲醛溶于硫酸中,得到C溶液;
称取硝酸镍溶于超纯水中,得到D溶液;
取WS2纳米材料用硝酸处理,得到E溶液;
将制备的A、B、C、D、E溶液按1:0.2~0.55:0.14~0.2:0.07~0.08:0.01比例混合,摇匀,即得该尿液羟苯衍生物检测试剂。
2.根据权利要求1所述的环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,制备B溶液所用的浓硝酸摩尔浓度为4.5moL/L。
3.根据权利要求1所述的环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,所述B溶液为硝酸亚汞溶液,其浓度为210~245g/L。
4.根据权利要求1所述的环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,制备C溶液所用的硫酸的摩尔浓度为10.7moL/L。
5.根据权利要求1所述的环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,所述C溶液为二甲氨基苯甲醛溶液,其浓度为3~5g/L。
6.根据权利要求1所述的环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,所述D溶液为硝酸镍溶液,其浓度为300~500g/L。
7.根据权利要求1所述的环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,制备E溶液所用的硝酸摩尔浓度为6mol/L。
8.根据权利要求1所述的环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,所述E溶液为纳米胶体溶液,其浓度为0.3~0.7g/L。
9.根据权利要求1所述的环保型尿液羟苯衍生物检测试剂的制备方法,其特征在于,WS2纳米材料的X射线衍射结果为六边形2H-WS2,粒径为1μm。
10.一种环保型尿液羟苯衍生物检测试剂,其特征在于,采用如权利要求1-9任一项所述的方法制备得到。
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