蒙药十八味欧曲丸中游离汞的含量测定

马蕊; 丁玉竹; 哈伟; 师彦平

doi:10.16495/j.1006-3757.2023.03.006

蒙药十八味欧曲丸中游离汞的含量测定

doi: 10.16495/j.1006-3757.2023.03.006

中国科学院兰州化学物理研究所，中国科学院西北特色植物资源化学重点实验室，甘肃省天然药物重点实验室，甘肃兰州　730000

基金项目: 内蒙古自治区科技转化项目

详细信息

作者简介:
马蕊（1996−），女，助理工程师，主要从事药物化学成分与分析技术研究，E-mail：marui13@licp.cas.cn

通讯作者:
哈伟（1984−），男，研究员，《分析测试技术与仪器》青年编委，主要从事中药化学成分与药物分析化学研究，E-mail: hawei2012@licp.cas.cn

师彦平（1965−），男，研究员，《分析测试技术与仪器》主编，主要从事药物化学成分与分析技术研究，E-mail：shiyp@licp.cas.cn

中图分类号: O657. 31
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- 被引次数: 0
出版历程
- 收稿日期: 2023-06-02
- 录用日期: 2023-08-28
- 修回日期: 2023-08-28
- 刊出日期: 2023-09-25

Determination of Dissociative Mercury in Mongolian Medicine Shibawei Ouqu Pills

Key Laboratory for Natural Medicine of Gansu Province, Key Laboratory of Chemistry of Northwestern Plant Resources, Chinese Academy of Sciences, Lanzhou Institute of Chemical Physics, Chinese Academy of Sciences, Lanzhou 730000, China

摘要

摘要: 建立特色蒙药十八味欧曲丸中游离汞的含量测定方法，为十八味欧曲丸质量标准中游离汞的限量检测提供技术支撑. 利用游离汞易溶于硝酸而炮制品不溶于硝酸的性质，以硝酸为溶剂提取，通过原子荧光光谱法对十八味欧曲丸中游离汞进行含量测定. 汞在0.1～2.0 μg/L范围内呈现良好的线性关系，回归方程为Y=1 467.197 6X+3.391 5，相关系数R²为0.999 59，平均回收率为95.0%，相对标准偏差（RSD）为4.436%（n=6），测得十八味欧曲丸中游离汞的平均质量分数为0.671 mg/g. 方法操作简单、结果准确可靠，可用作特色蒙药十八味欧曲丸质量标准提升研究中游离汞的限量测定.
- 十八味欧曲丸 /
- 游离汞 /
- 原子荧光光谱法 /
- 含量测定 /
- 限量检查
Abstract: The method for the determination of dissociative mercury contents in the characteristic Mongolian medicine Shibawei Ouqu pills was established, and the technical support for the limited detection of dissociative mercury in the quality standard of Shibawei Ouqu pills was provided. The dissociative mercury is easily soluble in nitric acid, while processed products are insoluble in nitric acid. Then, the content of dissociative mercury in Shibawei Ouqu pills was determined by atomic fluorescence spectrometry using nitric acid as the solvent. The dissociative mercury showed a good linear relationship in the range of 0.1~2.0 μg/L. The regression equation was Y=1 467.197 6X+3.391 5, and the correlation coefficient R² was 0.999 59, the average recovery was 95.0%, and relative standard deviation (RSD) was 4.436% (n=6). The average content of dissociative mercury in Shibawei Ouqu pills was 0.671 mg/g. The method is simple, accurate and reliable, and can be used for the limited determination of dissociative mercury in the study of quality standard improvement of Shibawei Ouqu pills.
- Shibawei Ouqu pills /
- dissociative mercury /
- atomic fluorescence spectrometry /
- content determination /
- limited determination

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图 1 汞标准曲线

Figure 1. Standard curve of mercury

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表 1 线性关系考察结果

Table 1. Results of linear relationship test

序号	质量浓度/（μg/L）	荧光强度
STD.01	0.1	132.000
STD.02	0.2	265.650
STD.03	0.5	729.160
STD.04	1.0	1 523.055
STD.05	2.0	2 917.535

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表 2 样品空白溶液试验结果

Table 2. Results of standard blank solution

序号	空白溶液荧光强度	空白溶液质量浓度/（μg/L）
1	24.190	0.014
2	15.685	0.008
3	17.668	0.010
4	15.250	0.008
5	19.053	0.011
6	21.325	0.012
7	21.195	0.012
8	21.260	0.012
9	20.735	0.012
10	18.790	0.010
11	20.658	0.012

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表 3 精密度试验结果

Table 3. Results of precision test

序号	标准溶液质量浓度/（μg/L）	所测荧光强度	质量浓度/ （μg/L）	RSD/%
1	0.500	730.304	0.493	1.448
2	0.500	731.869	0.494
3	0.500	752.216	0.507
4	0.500	730.304	0.493
5	0.500	728.739	0.492
6	0.500	758.477	0.511
7	0.500	730.304	0.493
8	0.500	728.739	0.492
9	0.500	736.565	0.497
10	0.500	727.174	0.491
11	0.500	744.390	0.502

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表 4 重复性试验结果

Table 4. Results of repetitive test

供试品质量/g	供试品质量浓度/（μg/L）	汞的质量分数/ （mg/g）	汞的平均质量分数/（mg/g）	RSD/%
0.100	69.523	0.695	0.668	2.674
0.100	64.994	0.650
0.100	68.132	0.681
0.100	67.157	0.672
0.100	64.968	0.650
0.100	66.240	0.662

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表 5 加标回收试验结果

Table 5. Results of spiked recovery test

序号	加标汞质量分数/（mg/g）	供试品质量/g	供试品质量浓度/（μg/L）	测得质量分数/ （mg/g）	平均质量分数/（mg/g）	回收率/%	平均回收率/%	RSD/%
1-1	0	0.100	69.293	0.693	0.682	–	–	1.941
1-2		0.100	66.908	0.669
1-3		0.100	67.916	0.679
1-4		0.100	69.106	0.690
1-5		0.100	66.646	0.665
1-6		0.100	69.841	0.697
2-1	0.7	0.100	133.104	1.330	1.343	92.6	95.0	4.436
2-2		0.100	131.912	1.316		90.0
2-3		0.100	132.681	1.326		92.0
2-4		0.100	134.833	1.345		94.7
2-5		0.100	137.139	1.369		98.1
2-6		0.100	139.986	1.394		101.7

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表 6 3批供试品测定结果（n=3）

Table 6. Results of 3 batches test materials (n=3)

样品批次编号	供试品质量/g	供试品质量浓度/（μg/L）	汞的质量分数/（mg/g）	平均值±SD/ （mg/g）
220505	0.100	71.792	0.716	0.692±0.022
	0.100	68.994	0.689
	0.100	67.480	0.672
220506	0.100	72.211	0.717	0.675±0.046
	0.100	68.677	0.684
	0.100	62.674	0.626
220507	0.100	61.871	0.618	0.646±0.037
	0.100	63.196	0.631
	0.100	69.095	0.688
平均值				0.671

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