泡腾片辅助提取结合罗丹明B型荧光探针快速检测粮食中的汞元素

张婧蕾; 张连钢; 牛列琴; 周鑫魁; 沈海波; 李建民; 方剑儒

doi:10.13386/j.issn1002-0306.2022080136

泡腾片辅助提取结合罗丹明B型荧光探针快速检测粮食中的汞元素

doi: 10.13386/j.issn1002-0306.2022080136

1.
甘肃省嘉峪关市食品药品和医疗器械检验检测中心，甘肃嘉峪关 735100
2.
中国铁路兰州局集团有限公司疾病预防控制所，甘肃嘉峪关 735100
3.
甘肃中商食品质量检验检测有限公司，甘肃兰州 730010
4.
甘肃省张掖市药品检验检测中心，甘肃张掖 734000

基金项目: 嘉峪关市科技局重点研发计划（20-32）。

详细信息

作者简介:
张婧蕾（1994−），女，硕士，助理工程师，研究方向：食品药品分析检验检测，E-mail：215687260@qq.com

通讯作者:
周鑫魁（1986−），男，硕士，高级工程师，研究方向：有机合成、分析检测，E-mail：664258985@qq.com

中图分类号: TS207.3
计量
- 文章访问数: 24
- HTML全文浏览量: 14
- PDF下载量: 2
- 被引次数: 0
出版历程
- 收稿日期: 2022-08-15
- 网络出版日期: 2023-05-22
- 刊出日期: 2023-07-01

Assisted Extraction Combined with Effervescent Tablets and Rhodamine B Fluorescence Probe for Rapid Detection of Elemental Mercury in Grain

1.
Jiayuguan City, Gansu Province Food Medicine and Medical Equipment Inspection and Testing Center, Jiayuguan 735100, China
2.
Institute for Disease Control and Prevention, China Railway Lanzhou Bureau Group Co., Ltd., Jiayuguan 735100, China
3.
Gansu Zhongshang Food Quality Test and Detection Co., Ltd., Lanzhou 730010, China
4.
Zhangye Pharmaceutical Inspection and Testing Center, Zhangye 734000, China

摘要

摘要: 为建立一种粮食中汞元素（Hg）的快速检测方法。自主合成罗丹明B型荧光探针，并利用功能离子液体作为探针体系的载体和生色基团。使原本的荧光探针体系，变成可见光探针体系。所建立的可见光探针体系与Hg结合，根据Hg含量的不同呈现不同深浅的玫红色。在550 nm波长下，样品中Hg含量0.5~20 ng/g范围内，显色的探针体系紫外吸光度与Hg含量成正比。结合泡腾片暴气辅助提取的方式，控制暴气反应的初始速度，减少暴气过程Hg的损失，达到准确定性定量检测的目的。该检测方法回收率90.98%~102.46%，精密度RSD为2.76%~4.76%，检出限1.0 ng/g。该快速检测方法具有高效、准确、灵敏度高、特异性强，适用范围广等优势。适用于谷物，小麦等粮食及其食品中汞元素的大批量筛查和检测工作。同时该方法和原理可以为可视化探针快速检测领域提供一定的参考和实验思路。
- 汞元素 /
- 粮食 /
- 快速检测 /
- 功能离子液体 /
- 可见光探针体系 /
- 泡腾片
Abstract: To establish a rapid method for determination of mercury in grain, Rhodamine type B fluorescent probe was synthesized and used as the carrier and chromogenic group of the probe system. The original fluorescent probe system was made into a visible light probe system, where this principle was used in conjunction with extraction assisted by effervescent tablets to establish a rapid method for the detection of elemental mercury (Hg) in grain. The initial speed of the blast reaction was controlled via the use of the bubble tablet blast method and the loss of Hg could be reduced in the course of the initial blast. After combining with different concentrations of Hg, the probe system make the originally colorless probe system turn into a rosy red color. The color developing probe system was in the range of 0.5~20 ng/g of Hg content in the sample at 550 nm, and the shade of color was proportional to the Hg content, whose range in the samples could also be assessed using a colorimetric card with naked eye. In the present study, the recoveries were 90.98%~102.46%, the precision RSD was 2.76%~4.76% and the detection limit was 1.0 ng/g. The rapid detection method has the advantages of high efficiency, accuracy, high sensitivity, specificity and wide applicability. Taken together, it is suitable for bulk screening and detection of elemental mercury in grains, wheat and other grains and their food products. Also, the method and principle might provide novel insights for the field of visualization probe rapid detection.
- elemental mercury /
- grain /
- rapid detection /
- functional ionic liquids /
- visible light probe system /
- effervescent tablets

HTML全文

图 1 样品前处理装置示意图

Figure 1. Schematic diagram of the sample pre-treatment device

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图 2 标准曲线各浓度点显色效果图

Figure 2. Schematic diagram of the sample pre-treatment device

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表 1 米粉样品，残留样品及溶液中汞含量检测结果

Table 1. Results of testing mercury content in rice flour samples, residual samples and solutions

样品序号	样品检测结果（ng/g）	残留米粉样品检测结果（ng/g）	氢汞气体产气效率（%）	气体发生器中溶液检测结果（ng/mL）	气体收集装置中溶液检测结果（ng/mL）	吸附效率（%）
米粉1号	1.29	0.104	92.94	0.00（未检出）	1.18	99.49
米粉2号	3.33	0.152	95.44	0.00（未检出）	3.15	99.12
米粉3号	9.84	0.225	97.71	0.00（未检出）	9.39	97.66

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表 2 米粉样品，接收液，离子液体中汞含量检测结果

Table 2. Results of testing mercury content in rice flour samples, receiving liquid and ionic liquid

样品序号	样品检测结果（ng/g）	离子液体萃取后气体发生器中溶液检测结果（ng/mL）	残留量（%）	未经离子液体萃取5 mL接收液中汞的理论含量（ng）	离子液体中汞的含量（ng）	吸附效率（%）
米粉1号	1.29	0.064	4.96	5.90	5.71	96.78
米粉2号	3.33	0.074	2.22	15.75	15.26	96.89
米粉3号	9.84	0.077	0.78	46.95	45.91	97.78

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表 3 方法的准确度及精密度

Table 3. The accuracy and precision of the method

样品序号	Hg含量质控理论值（ng/g）	本方法检测结果（ng/g）	回收率（%）	RSD （%）	ICP-MS 检测结果（ng/g）	回收率（%）	RSD （%）
米粉1号	1.22±0.21	1.24	101.64	4.76	1.06	86.89	2.89
		1.25	102.46		1.09	89.34
		1.17	95.90		1.12	91.80
		1.11	90.98		1.15	94.26
		1.15	94.26		1.11	90.98
		1.23	100.82		1.08	88.52
米粉2号	3.41±0.32	3.35	98.24	2.78	3.29	98.80	2.80
		3.26	95.60		3.31	99.40
		3.19	93.55		3.22	96.70
		3.29	96.48		3.34	100.30
		3.44	100.88		3.16	94.89
		3.22	94.43		3.11	93.39
米粉3号	10.11±0.68	10.25	101.38	2.76	9.28	91.79	2.80
		9.87	97.63		9.74	96.34
		10.12	100.10		9.68	95.75
		10.22	101.09		9.24	91.39
		9.78	96.74		9.53	94.26
		9.56	94.56		9.42	93.18

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表 4 方法的检出限

Table 4. The detection limit of the method

20份阴性面粉样品吸光度
0.0021	0.0018	0.0027	0.0022	0.0019
0.0014	0.0015	0.0012	0.0021	0.0016
0.0024	0.0023	0.0014	0.0019	0.0021
0.0020	0.0025	0.0019	0.0017	0.0013
标准偏差（噪声）			0.00049
5倍噪声			0.00245
最低检测浓度理论值（ng/mL）			0.44

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表 5 检出限验证结果

Table 5. Detection limit verification result

样品序号	加标浓度（ng/g）	检测结果（ng/g）	回收率（%）	RSD（%）
1号加标样品	0.5	0.33	66.00	32.05
		0.61	122.00
		0.41	82.00
2号加标样品	1.0	0.95	95.00	7.36
		0.90	90.00
		1.04	104.00

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表 6 泡腾片辅助提取对比结果

Table 6. Extraction and comparison of effervescent tablets

样品序号	Hg含量理论值（ng/g）	ICP-MS 检测结果（ng/g）	本方法检测结果（ng/g）	本方法不使用泡腾片检测结果（ng/g）
米粉1号	1.22±0.21	1.08	1.11	0.74
米粉2号	3.41±0.32	3.21	3.26	2.54
米粉3号	10.11±0.68	9.58	9.77	8.14

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表 7 干扰离子对检测方法的影响

Table 7. The effect of interfering ions on the detection method

干扰离子加标量（ng/g）	汞离子加标量（ng/g）	显色现象	实测浓度（ng/g）	回收率（%）	RSD （%）
2.0	2.0	微红色	1.91	95.5	3.40
		微红色	1.85	92.5
		微红色	1.98	99.0
10.0		微红色	2.04	102.0	4.21
		微红色	2.11	105.5
		微红色	1.94	97.0
50.0		微红色	1.84	92.0	7.88
		微红色	1.96	98.0
		微红色	2.15	107.5

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