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

Abstract

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

CLC Number:

TQ658.4

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.

Figures/Tables 9

Tab. 1

Tab. 2

Fig. 1

Fig. 2

Fig. 3

Fig. 4

Tab. 3

Fig. 5

Tab. 4

References 9

[1]	Kakar A, Newby E E, Kakar K, et al. A randomised clinical trial to access maintenance of gingival health by a novel dentifrice containing 0.1%w/w o-cymene-5-ol and 0.6%w/w zinc chloride[J]. International Dental Journal, 2011(S3):13-20.
[2]	Xie Xiaofang, Chen Minshan, Li Lin. Application of grapefruit extract/o-cymene-5-ol in toothpaste and evaluation of its sterilization rate[J]. Oral Care Industry, 2017,27(1): 21-24.
[3]	Chen Wenjie, Chen Zhaobin, Xie Yuting. Study on disinfection effect of o-cymen-5-ol on Staphylococcus aureus[J]. Chinese Journal of Disinfection, 2019,36(2): 99-103.
[4]	Chen Minshan, Li Lin, Li Ping. Study on bacteriostasis of natural extract and its application in oral care products[J]. Oral Care Industry, 2016,26(4): 16-20.
[5]	The Cosmetic Ingredient Review. Final report on the safety assessment of o-cymen-5-ol [R/OL]. (1984) [2020-01-03]. https://online.personalcarecouncil.org/ctfa-static/online/lists/cir-pdfs/pr207.pdf.
[6]	Andersen A. Final report on the safety assessment of sodium p-chloro-m-cresol, p-chloro-m-cresol, chlorothymol, mixed cresols, m-cresol, o-cresol, p-cresol, isopropyl cresols, thymol, o-cymen-5-ol, and carvacrol[J]. International Journal of Toxicology, 2006,25(S1):29-127. doi: 10.1080/10915810600716653
[7]	Sun Zongxi, Lv Xiaohui, Xu Guihua, et al. Chemical constituents of volatile oil from different parts of bupleurum chinese in gansu by GC-MS[J]. Chinese Journal of Experimental Traditional Medical Formulae, 2012,18(9): 75-78.
[8]	Wang Juan, Yu Wen. Determination of 3-methyl-4-isopropyl phenol in hand cleanser by high performance liquid chromatography[J]. China Cleaning Industry, 2016,11:38-41.
[9]	Xia Zemin, Liang Wenyao, Mo Tingyuan, et al. Determination of 4-isopropyl-m-cresol in cosmetics by high performance liquid chromatography[J]. Chemical Analysis and Meterage, 2019,28(2): 76-78.

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

[1]	Liyuan Zhang, Linqi Yan, Qiaoyuan Cheng, Lvye Qi, Rong Wang, Liuqian Huang. Determination of 14 kinds of α-hydroxy acids and hydroxy esters in cosmetics [J]. China Surfactant Detergent & Cosmetics, 2024, 54(3): 353-359.
[2]	Yixiang Lu, Liting Wu, Jimin Jiang, Hailu Chen, Xuan Huang. Determination of tolnaftate and liranaftate in cosmetics by high performance liquid chromatography and verification by high performance liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2024, 54(2): 231-238.
[3]	Liyuan Zhang, Qiaoyuan Cheng, Cen Chen, Zehua Li, Liuqian Huang, Lvye Qi. Determination of 3 kinds of α-hydroxy acids and their esters in cosmetics by high performance liquid chromatography [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 102-106.
[4]	Linling Lu, Hui Lu, Chunyan Min, Yefei Qian. Determination of functional components of Glycyrrhizae, Ginseng and Scutellariae in facial masks by UHPLC-MS/MS [J]. China Surfactant Detergent & Cosmetics, 2024, 54(1): 107-113.
[5]	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.
[6]	Wang Jicai, Jian Ruidong, Xie Yu, Chen Xiaobin, Zhou Yi, Tan Jianhua. Study on the standardization of evaluation for the efficacy of toothpaste in extrinsic stain removal [J]. China Surfactant Detergent & Cosmetics, 2023, 53(9): 1101-1107.
[7]	Zhou Lei,Cao Dongxia,Li Jiahong,Su Nafeng,Li Wenhui. Study of different forms of fluoride in toothpaste by solid state NMR [J]. China Surfactant Detergent & Cosmetics, 2023, 53(8): 963-967.
[8]	Liu Ying, Lin Min, Dai Sirui. Simultaneous determination of nine effective components in Polygonum Multif lorum Fangtuoyufa Jinghuaye by HPLC-QAMS [J]. China Surfactant Detergent & Cosmetics, 2023, 53(7): 841-848.
[9]	Sun Xiaojie, Wang Yumei, Liu Zhen, Liu Qinan. Determination of 17 cephalosporins residues in cosmetics by HPLC-MS-MS [J]. China Surfactant Detergent & Cosmetics, 2023, 53(6): 714-720.
[10]	Jiang Chengjun, Wu Zhishan, Yin Shuai, Huang Haiping. Determination of 33 kinds of components such as caffeine in bodybuilding products by liquid chromatography-tandem mass spectrometry [J]. China Surfactant Detergent & Cosmetics, 2023, 53(5): 588-595.
[11]	Li Zexiaqiong, Qiu Hongyan, Ma Ying, Liu Dan, Zhao Li. Simultaneous determination of caprylhydroxamic acid, 4-hydroxyacetophenone and p-anisic acid in cosmetics by HPLC-MS [J]. China Surfactant Detergent & Cosmetics, 2023, 53(5): 596-601.
[12]	Zhuo Wenshan, Feng Shunqing, Tang Jianfeng. Determination of sodium lauroyl glycinate by HPLC-ELSD [J]. China Surfactant Detergent & Cosmetics, 2023, 53(2): 220-225.
[13]	Gao Yan, Chen Jiewen, Xiao Lei. Study on the rheological properties of toothpastes from different production processes [J]. China Surfactant Detergent & Cosmetics, 2023, 53(11): 1299-1304.
[14]	Zheng Lixia, Gao Huiqin, Li Sa, Guo Congjia, Hao Qianying, Wu Guotai. Determination of ferulic acid and baicalin content in Gui Qin toothpaste and its pharmacodynamic study [J]. China Surfactant Detergent & Cosmetics, 2023, 53(11): 1345-1350.
[15]	Pan Jifei, Wang Xiaona, Guo Haijiao, Yang Suzhen, Chen Jianying. The establishment and application of an in vitro evaluation system for 5α-reductase inhibitors [J]. China Surfactant Detergent & Cosmetics, 2023, 53(11): 1280-1284.

Research on the determination of o-cymene-5-ol in oral care and cleansing products by HPLC

RichHTML

PDF (PC)

Like

Knowledge

Abstract

Cite this article

share this article

Figures/Tables 9

References 9

Related Articles 15

Metrics

Comments

Recommended 10