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日用化学工业（中英文）

日用化学工业（中英文） ›› 2026, Vol. 56 ›› Issue (1): 122-128.doi: 10.3969/j.issn.2097-2806.2026.01.015

• 分析与检测 • 上一篇    下一篇

高效液相色谱法同时测定口腔护理牙膏中5种新型防腐剂含量

谢冰冰1,刘琳立2,范丽敏1,*()   

  1. 1.濮阳医学高等专科学校 护理学院， 河南 濮阳 457000
    2.坦波夫国立大学， 俄罗斯 坦波夫 坦波夫州 392036
  • 收稿日期:2025-04-08 修回日期:2026-01-05 出版日期:2026-01-22 发布日期:2026-02-05

Simultaneous determination of 5 new preservatives in oral care toothpaste by high performance liquid chromatography

Bingbing Xie1,Linli Liu2,Limin Fan1,*()   

  1. 1. School of Nursing, Puyang Medical College, Puyang, Henan 457000, China
    2. Tambov State University, Tambov Oblast, Tambov 392036, Russia
  • Received:2025-04-08 Revised:2026-01-05 Online:2026-01-22 Published:2026-02-05
  • Contact: E-mail: fanlimin29723@163.com.

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摘要：

建立了HPLC同时测定口腔护理牙膏中5种新型防腐剂（乙基己基甘油、1, 2-己二醇、1, 2-戊二醇、1, 3-辛二醇、1, 2-辛二醇）含量的方法。以甲醇-水（体积比7∶3）作为牙膏提取试剂，40 ℃下超声处理20 min（功率300 W），超声后以10 000 r/min离心10 min，取上清液经0.22 μm有机系滤膜过滤。采用Oasis HLB固相萃取柱净化样品。配备Agilent G1315D二极管阵列检测器的Agilent 1260 Infinity HPLC系统进行分析。选择耐酸性Agilent ZORBAX Eclipse Plus C18色谱柱，柱温35 ℃。流动相为水（含0.1%甲酸）-甲醇。检测波长为210 nm。结果显示，该方法的日内RSD均低于4%，日间RSD均低于5%，表明该方法具有良好的精密度；线性回归分析显示，5种新型防腐剂的线性范围为0.1~200 μg/mL，r值在0.999 1~0.999 5区间，检测限为0.05~0.08 μg/mL，定量限为0.15~0.25 μg/mL，表明该方法线性关系良好，具有较高的适用性；5种新型防腐剂的加标回收率在95.56%~104.94%之间，RSD值均低于5%（1.63%~4.45%）。应用该方法测定了32种牙膏中5种新型防腐剂的含量，在4种牙膏检测出乙基己基甘油，在2种牙膏中检测出了1, 2-己二醇。总之，该方法在同时检测牙膏中5种新型防腐剂时具有良好的精密性、适用性和准确性。

关键词: 口腔护理牙膏, 高效液相色谱法, 同时测定, 新型防腐剂

Abstract:

A method for the simultaneous determination of the contents of five new preservatives （ethylhexylglycerin, 1,2-hexanediol, 1,2-pentanediol, 1,3-octanediol, and 1,2-octanediol） in oral care toothpaste by high performance liquid chromatography （HPLC） was established. Methanol-water （volume ratio 7∶3） was used as the extraction reagent for toothpaste. The samples were subjected to ultrasonic treatment at 40 ℃ for 20 min （power 300 W）, followed by centrifugation at 10 000 r/min for 10 min. The supernatant was filtered through a 0.22 μm organic filter membrane. The samples were purified using an Oasis HLB solid-phase extraction column. Analysis was performed on an Agilent 1260 Infinity HPLC system equipped with an Agilent G1315D diode array detector. An acid-resistant Agilent ZORBAX Eclipse Plus C18 chromatographic column was selected, with the column temperature set at 35 ℃. The mobile phase consisted of water （containing 0.1% formic acid） and methanol. The detection wavelength was 210 nm. The results show that the intraday relative standard deviation （RSD） of the method is all less than 4%, and the interday RSD is all less than 5%, indicating good precision of the method. Linear regression analysis reveals that the linear range of the five new preservatives is 0.1-200 μg/mL, with the correlation coefficients （r） ranging from 0.999 1 to 0.999 5, limits of detection （LOD） from 0.05 to 0.08 μg/mL, and limits of quantification （LOQ） from 0.15 to 0.25 μg/mL, demonstrating a good linear relationship and high applicability of the method. The spiked recoveries of the five new preservatives range from 95.56% to 104.94%, with all RSD values below 5% （1.63%-4.45%）. This method is applied to determine the contents of the five new preservatives in 32 types of toothpaste. Ethylhexylglycerin is detected in 4 types of toothpaste, and 1,2-hexanediol is detected in 2 types of toothpaste. In conclusion, this method exhibits good precision, applicability, and accuracy for the simultaneous determination of the five new preservatives in toothpaste.

Key words: oral care toothpaste, high performance liquid chromatography, simultaneous determination, new preservative

中图分类号: 

  • TQ658