牙膏中可溶性/游离氟化物快速定量分析方法研究

doi:10.3969/j.issn.2097-2806.2024.01.005

摘要/Abstract

摘要：

有效结合低场核磁共振技术（LF-NMR）和高场固体核磁共振技术（SS-NMR），系统研究了牙膏中氟化物，建立了牙膏中可溶性/游离氟化物的LF-NMR快速定量分析方法。实验结果表明，LF-NMR 6次平行测试的相对标准偏差RSD均在2%以内，精密度高。实际样品测试中，117款牙膏样品中有110款样品LF-NMR定量分析数据与国标方法氟离子选择电极法测试数据相对偏差在±5%以内;另有7款样品，LF-NMR与国标方法定量数据有较大的差异，结合SS-NMR的氟化物物种及形态分析结果，发现造成差异的主要原因是体系中存在不溶性氟化物物种，影响整个体系的弛豫时间，造成LF-NMR测试结果较国标方法低，但LF-NMR可作为快筛手段及时反映牙膏质量问题。LF-NMR方法前处理简单，牙膏样品无需任何前处理，直接装样测试，整个测试流程5 min左右，是非常快速的定量分析手段，并且，结合SS-NMR技术，进一步明确了LF-NMR定量测试适用体系。

关键词: 快速定量, 牙膏, 氟化物, 低场核磁共振技术, 固体核磁共振技术

Abstract:

Low-field nuclear magnetic resonance （LF-NMR） and high-field solid-state nuclear magnetic resonance （SS-NMR） were effectively combined to systematically study the fluoride in toothpastes, and a rapid LF-NMR method for quantitative analysis of soluble/ionic fluoride in toothpastes was established. The results showed that the relative standard deviations （RSDs） of LF-NMR in 6 parallel tests were all within 2%, indicative of high precision. In the actual sample test, 117 toothpaste samples were selected, and the relative deviation between LF-NMR data and national standard test data was within±5% for the 110 toothpaste samples therein. For the other 7 samples, the quantitative data of LF-NMR were significantly different from that of the national standard method. Combined with the analysis results of SS-NMR, it was found that the difference was due to the existence of insoluble fluoride substances in the system, which affected the relaxation time of the whole system and therefore the results of LF-NMR were lower than that of the national standard method. Nevertheless, LF-NMR could still be used as a fast screening method to reflect the quality of toothpaste in time. The LF-NMR method was a very fast quantitative analysis method, the toothpaste samples could be directly tested without any pre-treatment, and the whole test process was approximately 5 min. In addition, combined with SS-NMR technology, the systems which were applicable to be measured with LF-NMR quantitative test were further defined.

Key words: rapid quantification, toothpaste, fluoride, low field nuclear magnetic resonance, solid state nuclear magnetic resonance

中图分类号:

TQ658

曹东霞, 周雷, 李家宏, 林长钦, 陈锦玲. 牙膏中可溶性/游离氟化物快速定量分析方法研究[J]. 日用化学工业（中英文）, 2024, 54(1): 38-44.

Dongxia Cao, Lei Zhou, Jiahong Li, Changqin Lin, Jinling Chen. Rapid quantitative analysis of soluble/ionic fluoride in toothpastes[J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 38-44.

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参考文献 14

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检测样品	氟化物和摩擦剂配方	样品数量
1	氟化钠和水合硅石	67
2	单氟磷酸钠和水合硅石	40
3	单氟磷酸钠和碳酸钙	7
4	单氟磷酸钠和磷钙粉	3

样品	氟化物种类	测定值1/ （mg/kg）	测定值2/ （mg/kg）	测定值3/ （mg/kg）	测定值4/ （mg/kg）	测定值5/ （mg/kg）	测定值6/ （mg/kg）	RSD/%
1	NaF	962	950	953	938	942	930	1.21
2	NaF	1 405	1 401	1 408	1 410	1 374	1 410	0.97
3	NaF	1 039	1 045	1 056	1 040	1 035	1 029	0.89
4	MPF	596	580	574	596	578	592	1.70
5	MPF	771	794	801	771	786	801	1.76
6	MPF	929	930	915	910	920	912	0.93

序号	电极法/ （mg/kg）	LF-NMR/（mg/kg）	相对偏差/%	标识值
1	555	411	-26.0	950
2	891	659	-26.0	1 000
3	1 159	899	-22.4	1 500
4	823	426	-48.3	1 000
5	459	361	-21.3	900
6	1 090	224	-79.4	1 450
7	1 123	301	-73.2	1 450

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