高效液相色谱法测定口腔清洁护理用品中o-伞花烃-5-醇含量的研究

doi:10.3969/j.issn.1001-1803.2020.11.013

摘要/Abstract

摘要：

建立用高效液相色谱法测定牙膏、漱口水等口腔清洁护理用品中o-伞花烃-5-醇含量的方法。样品用50%甲醇水溶液溶解,经磁力搅拌、超声提取、离心分离及过滤处理,以Dionex Acclaim^TM 120型C₁₈为色谱柱,乙腈-10 mmol/L磷酸二氢钾为流动相进行梯度洗脱,流量为1.5 mL/min,柱温为30 ℃,采用二极管阵列检测器进行检测,检测波长为279 nm,外标法定量。研究结果表明,o-伞花烃-5-醇在1.00~15.0 mg/L的质量浓度范围内与其峰面积具有良好的线性关系,R²=0.999 9,方法的检出限为20 mg/kg,定量限为60 mg/kg,样品加标回收率为96.3%~101.4%,测定结果的相对标准偏差为0.41%~1.63% （n=6）。该方法具有操作简便、灵敏度高、重现性好等特点,适用于口腔护理产品中o-伞花烃-5-醇的定性定量分析。

关键词: o-伞花烃-5-醇, 抑菌, 限用物质, 高效液相色谱法, 牙膏

Abstract:

A reversed-phase high performance liquid chromatographic method was developed for the determination of o-cymene-5-ol in oral care and cleansing products such as toothpastes and mouthwash. Samples were extracted by 50% methanol aqueous solution, and preprocessed by magnetic stirring, ultrasonic extraction, centrifugation and filtration. Dionex Acclaim ^TM 120 C₁₈ was used as a chromatographic column and acetonitrile-10 mmol/L monopotassium phosphate as mobile phase for gradient elution. The flow rate was 1.5 mL/min, and the column temperature was 30 ℃. The detection was carried out by a diode array detector with the wavelength of 279 nm. The external standard method was used for quantitative analysis. The mass concentration of o-cymene-5-ol in the range of 1.00-15.0 mg/L shows a good linear relationship with the peak area. The correlation coefficient is 0.999 9, the detection limit is 20 mg/kg and the quantitative limit is 60 mg/kg. The recovery rate is 96.3%-101.4%, and the relative standard deviation is 0.41%-1.63% （n=6） . The method is simple, sensitive and reproducible. It is suitable for the determination of o-cymene-5-ol in oral care and cleansing products.

Key words: o-cymene-5-ol, antimicrobial, restricted substance, HPLC, toothpaste

中图分类号:

TQ658.4

施裔磊. 高效液相色谱法测定口腔清洁护理用品中o-伞花烃-5-醇含量的研究[J]. 日用化学工业, 2020, 50(11): 809-814.

SHI Yi-lei. Research on the determination of o-cymene-5-ol in oral care and cleansing products by HPLC[J]. China Surfactant Detergent & Cosmetics, 2020, 50(11): 809-814.

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参考文献 9

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时间/min	流量/（mL·min^-1）	φ（10 mmol/L磷酸二氢钾）/%	φ（乙腈）/%
0	1.5	62.0	38.0
16.00	1.5	62.0	38.0
17.00	1.5	30.0	70.0
27.00	1.5	30.0	70.0
28.00	1.5	62.0	38.0
35.00	1.5	62.0	38.0

甲醇含量/%	对照品溶解性	牙膏试样分散情况
0	不溶	易分散
10	极微溶解	易分散
20	极微溶解	易分散
50	略溶	易分散
70	略溶	难分散
100	溶解	难分散

牙膏名称	添加水平/（μg·g^-1）	实际加标量/（mg·kg^-1）	测得量/（g·g^-1）	回收率/%
阴性牙膏试样① （碳酸钙基质）	100	96.83	98.09	101.30
	200	193.66	196.34	101.39
	400	387.32	389.01	100.44
阴性牙膏试样② （二氧化硅基质）	100	96.83	96.80	99.97
	200	193.66	194.01	100.18
	400	387.32	388.49	100.30
阴性牙膏试样③ （磷酸氢钙基质）	100	96.83	95.30	98.42
	200	193.66	192.05	99.17
	400	387.32	387.78	100.12

实验室序号	标准曲线相关系数R²	检出质量浓度/（g·L^-1）	定量质量浓度/（g·L^-1）	加标回收率范围/%	某市售牙膏样品中o-伞花烃-5-醇的测得量/（mg·kg^-1）	RSD/% （n=6）
1	0.999 7	0.000 1	0.000 3	97.5~99.7	439	1.24
2	0.999 9	0.000 2	0.000 6	97.1~99.3	459	0.41
3	0.999 9	0.000 1	0.000 3	96.3~100.9	445	1.06
4	0.999 9	0.000 1	0.000 3	98.4~101.4	440	1.63
实验室间RSD/%					2.06

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