Determination of Organic Fluorinated Amines in Oral Care Products by Ultra Performance Liquid Chromatography-Charged Aerosol Detector Coupled with Solid-Phase Extraction
10.19756/j.issn.0253-3820.241105
- VernacularTitle:固相萃取-超高效液相色谱-电雾式检测器测定口腔护理用品中的有机氟化胺
- Author:
Xiao-Fang LI
1
;
Yan PENG
;
Di XIN
;
Wei ZHOU
;
Xiao-Hong QIAO
;
Hua-Jin SHI
;
Lei ZHANG
;
Guo-Qiang CAI
;
Ying LIU
Author Information
1. 纳爱斯浙江科技有限公司,杭州 310056;浙江省绿色清洁技术及洗涤用品重点实验室,丽水 323000
- Keywords:
Ultra performance liquid chromatography-charged aerosol detector;
Solid-phase extraction;
Olaflur;
Oral care products
- From:
Chinese Journal of Analytical Chemistry
2025;53(8):1362-1370,中插100-中插105
- CountryChina
- Language:Chinese
-
Abstract:
The major components of Olaflur raw material were characterized using ultra performance liquid chromatography-quadrupole time-of-flight-mass spectrometry(UPLC-Q-TOF/MS).The results revealed that cetyl amine fluoride(C16-AmF),octadecene amine fluoride(C18:1-AmF),and octadecyl amine fluoride(Olaflur)were the main components.The contents of C16-AmF,C18:1-AmF,and Olaflur in oral care products were determined via ultra performance liquid chromatography-charged aerosol detector coupled with solid-phase extraction(SPE-UPLC-CAD).The oral care sample was dispersed evenly with a 50%ethanol aqueous solution,and then vortexed with ethanol.The supernatant was collected by centrifugation,concentrated to near dryness,and redissolved with ultrapure water.The re-dissolved sample was loaded onto a Poly-Sery HLB Pro SPE column for purification and elution.The acetonitrile eluate was collected and concentrated to 1.0 mL.Finally,a prepared test solution was separated on a Thermo Acclaim Surfactant Plus chromatographic column(2.1 mm×150 mm,3 μm).Acetonitrile and 100 mmol/L acetic acid-ammonium acetate aqueous solution(pH=4.8)were used as the mobile phases for gradient elution.The flow rate was 0.3 mL/min and cloumn temperature was maintained at 40℃.The sample was detected using a charged aerosol detector,and quantified using an external standard method.The experimental results indicated that the three organic fluorinated amines showed good linear relationship in their respective concentration ranges.The correlation coefficients(r)were greater than 0.99.The limit of detection(LOD)and the limit of quantification(LOQ)of C16-AmF were 2.0 and 8.0 μg/mL,respectively.The LOD and LOQ of C18:1-AmF were 2.0 and 8.0 μg/mL,respectively.The LOD and LOQ of Olaflur were 3.0 μg/mL and 10.0 μg/mL,respectively.The spiked recoveries of the three organic fluorinated amines were 84.3%-104.2%,with relative standard deviations(RSDs)of 4.93%-5.82%.The 28 batches of commercial oral care samples were detected by this method and the results indicated that three organic fluorinated amines were detected in 18 samples and the total content were 22.2-11477.8 μg/g.This method had high sensitivity and good reproducibility.It was suitable for verifying the authenticity of the claims of oral care products promoted with Olaflur as the main efficacy ingredient and selling point,and provided a valuable reference for establishing and improving the standard analytical method for Olaflur.
