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| Simultaneous Determination of 19 Organic Antibacterial Agents in Tissue Paper and Paper Products by High Performance Liquid Chromatography |
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| DOI： |
| KeyWord:high performance liquid chromatography tissue paper and products organic antibacterial agent chlorophenol quaternary ammonium p-hydroxybenzoic acid esters |
| Author | Institution |
| QI Yan，LI Jin-qing，CHEN Man-ying，WU Shang-sen，TANG Chu-lin，LIU De-qun |
Guangdong Testing Institute of Product Quality Supervision， Foshan ， China |
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| Abstract: |
| In order to prevent the mildew of tissue paper and paper products， organic antibacterial agents are often used in the process of production, processing and storage. After a long-term accumulation and reaching a certain amount， the harm of the organic antibacterial agents to the environment and human body can not be ignored. However, there are few methods to detect a variety of organic antibacterial agents in tissue paper and paper products. A high performance liquid chromatographic（HPLC） method was established for the simultaneous extraction and determination of 19 organic antibacterial agents， including seven kinds of chlorophenols， six kinds of quaternary ammoniums and six kinds of p-hydroxybenzoic acid esters in tissue paper and paper products. The samples were firstly extracted twice with methanol containing 0.5% formic acid， then centrifuged at 9 000 r/min for 3 min and suctioned filtration with buchner funnel to collect filtrate. The filtrate was evaporated at 45 ℃ and condensed into about 1 mL， and then dried with nitrogen， dissolved with 2.0 mL methanol－water solution（1∶1， by volume）. 19 organic antibacterial agents were separated on a Welch Ultimate AQ C18 column（250 mm ×4.6 mm， 5 μm） by gradient elution， with methanol, acetonitrile and 0.05% phosphoric acid solution（containing 0.475 3 g tetrabutylammonium hydrogen sulfate） as mobile phases， then detected with photo-diode array detector（PDAD） at 191－400 nm. Results indicated that the calibration curves of chlorophenols， quaternary ammoniums and p-hydroxybenzoic acid esters showed good linear relationships in the ranges of 0.05－20 mg/L， 0.1－20 mg/L and 0.02－50 mg/L， respectively， with their correlation coefficients(r) not less than 0.996 0. The limits of detection(LOD， S/N ≥ 3) for 19 organic antibacterial agents were in the range of 0.05－0.3 mg/kg. The average recoveries of this method ranged from 74.8% to 101% with relative standard deviations(RSD， n=6) of 2.2%－5.6%. The developed method was used to evaluate the 19 organic antibacterial agents in wet tissue， facial tissue and paper cups. The results showed that the 19 organic antibacterial agents were not detected in facial tissue and paper cups. Chlorophenols were not found in wet tissue， but methyl 4-hydroxybenzoate was detected in two batches of wet tissue， with contents of 11.3 mg/kg and 15.4 mg/kg， respectively. Benzethonium chloride was detected in one batch of wet tissue， and the content was 132.3 mg/kg. Benzethonium chloride and cetylpyridinium chloride were simultaneously detected in one batch of wet tissues， and the contents were 152.2 mg/kg and 246.5 mg/kg， respectively. Therefore， the method is simple， rapid， accurate and reliable， and could be used to identify and detect 19 organic antibacterial agents in tissue paper and paper products. |
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