Determination of Benzalkonium Chloride Homologs in Complex Chemical Disinfectant by High-Performance Liquid Chromatography

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1 December 2011 ROCK A MINERAL ANALYSIS Vol. 30 No ~ * Platisil ODS 5 μm 250 mm 4. 6 mm mol /L 1% V /V ph = nm ~ 5 mg /ml ~ 10 mg /ml ~ 10 mg /ml mg / ml mg /ml mg /ml % ~ % RSD 2. 0% Determination of Benzalkonium Chloride Homologs in Complex Chemical Disinfectant by High-Performance Liquid Chromatography LIU Wen-wen ZHANG Jin QIAO Jun-qin LIAN Hong-zhen * State Key Laboratory of Analytical Chemistry for Life Science School of Chemistry & Chemical Engineering and Center of Materials Analysis Nanjing University Nanjing China Abstract An ion pair reversed phase High-Performance Liquid Chromatography HPLC method has been developed for the simultaneous determination of benzalkonium chloride BAC homologues dodecyl dimethyl benzyl ammonium chloride C 12 tetradecyl dimethyl benzyl ammonium chloride C 14 and cetyl dimethyl benzyl ammonium chloride C 16 in complex chemical disinfectant. Separation was carried out on Platisil ODS column 5 μm 250 mm 4. 6 mm using methanol and 200 mmol / L hexane sulfonate sodium aqueous solution consisting of 1% triethylamine V /V adjusted with perchloric acid to ph V /V as the mobile phase in an isocratic elution. The detection wavelength was 220 nm. In the experiment sodium hexanesulfonate was used as the ion-pair reagent to enhance the retention of benzalkonium chloride and triethylamine was used as the tailing-suppressor to restrain the adsorption of benzalkonium chloride to the residual silanols on the stationary phase surface. Calibration curves for C 12 C 14 and C 16 were linear in the range of mg /ml mg /ml and mg /ml with the limits of quantifications LOQs being and mg /ml respectively. The method presents excellent accuracy CB CB lww1102@ gmail. com hzlian@ nju. edu. cn 677

2 http www. ykcs. ac. cn 2011 and satisfactory precision and it has a significant advantage in the detection of low content samples. The average recoveries were in the range of 99. 3% % and the intra- and inter-day relative standard deviations RSDs were not more than 2. 0% for the determined compounds in benzalkonium chloride disinfectant and benzalkonium chloride towelette. Key words benzalkonium chloride complex chemical disinfectant ion pair revered phase high-performance liquid chromatography benzalkonium chloride BAC C 12 HPLC - MS 3 HPLC n - C 12 H 25 n - C 14 H 29 n - C 16 H 33 3 C 12 C 14 C Agilent 1200 Agilent 0. 1% ~ 0. 8% 1 DAD - SevenEasy ph S g /L 1. 2 HPLC Merck 98% Sigma HPLC USP 32 Tedia HClO 4 40% 20% 70% 99% Aladdinzh CE HPLC cm 6 cm 4 - HPLC - MS % C 12 - / - C 14 C g 25 ml mol /L 1% V /V HClO 4 ph = mg /ml mg /ml 678

3 mg /ml mg /ml ml 10 ml 5 C 12 C 14 C ml 4 ml 10 min 10 ml 2 ml 10 min 10 ml 10 ml ml 3 10 ml 1 mg /ml ml ml ml ml 0. 1 mg /ml ml ml ml 3 ml 2 ml 1 ml μm 1. 4 HPLC Platisil ODS C 18 5 μm 250 mm 4. 6 mm mol /L 1% V /V ph = V /V μm 1. 0 ml /min 220 nm 5 μl a C 12 C 14 C min min min C 12 R ~ 5 mg /ml 4 N + SiO - y = x S /N = mg /ml C ~ 10 mg /ml y = 2236x S /N = mg /ml C ~ 10mg /ml RSD 0. 7% 0. 8% 1. 4% 1 Fig. 1 Chromatograms of mixed benzalkonium chloride standard and benzalkonium chloride sample solutions a 0. 1 mg /ml b c 0. 1 mg /ml d e 0. 1 mg /ml 1 C 12 2 C 14 3 C y = x S /N = mg /ml ~

4 http www. ykcs. ac. cn 2011 SiO - R 4 N + ph % ph 0. 1% ph = 6. 0 ph = 6. 0 ph mmol /L 0. 1 mol /L mol /L mol /L 2 Fig. 2 Effect of concentration of hexane sulfonate sodium on retention time % 0. 2 mol /L ph = % 2. 0% % % 3 1% ph 85% 85% 0. 2 mol /L 1% ph 85% 680

5 nm 1 R 99. 3% ~ 205 nm % 220 nm RSD 2. 0% 1 Table 1 1 Recoveries of BAC homologs in benzalkonium chloride disinfectant and benzalkonium chloride towelette ρ B / mg ml - 1 RSD /% R /% R /% ρ B / mg ml - 1 RSD /% R /% R /% C C C Table 2 Determination of dodecyl dimethyl benzyl ammonium chloride and tetradecyl dimethyl benzyl ammonium chloride in benzalkonium chloride disinfectant and benzalkonium chloride towelette C 12 C 14 ρ / mg ml - 1 RSD /% ρ / mg L - 1 RSD /% ρ / mg ml - 1 RSD /% ρ / mg L - 1 RSD /% C Ferrer I Furlong E T. Identification of alkyl dimethylbenzylammonium surfactants in water samples by solid-phase extraction mol /L 1% ph = nm followed by ion trap LC/MS and LC/MS/MS J. Environmental Science & Technology The United States Pharmacopeia-National Formulary. United States Pharmacopeia USP32-NF27 M. United States 681

6 http www. ykcs. ac. cn 2011 Pharmacopeial Convention M. followed by on-line solid-phase extraction coupled to ion trap LC / MS / MS for analysis of benzalkonium chloride in 4. sediment samples J. Analytical Chemistry 2002 J J. benzalkonium chloride on skin by flow injection ion spray M M. Determination of residues of quaternary ammonium disinfectants in food products by liquid chromatography tandem mass spectrometry J. Journal of AOAC J. International ISO 2871 Surface active agents -detergents -determination of cationic-active matter content-part 2 Cationic-active matter of low molecular mass between 200 and 500 S ISO 2271 Surface active agents-detergents-determination of anionic-active matter by manual or mechanical direct twophase titration procedure S BS 3762 Analysis of formulated detergents Part-2 Qualitative test methods S Prince S J McLaury H J Allen L V McLaury P. Analysis of benzalkonium chloride and its homologs HPLC versus HPCE J. Journal of Pharmaceutical and Biomedical Analysis Turnes - Carou I Prieto - Blanco C Lopez - Mahia P Muniategui-Lorenzo S Practa-Roctrfguez D. Simultaneous separation of amidoamines and benzalkonium chloride surfactants by capillary zone electrophoresis J. Chromatographia / J J. J Tavlarakis P Greyling J Snow N H. Simultaneous determination of pramoxine HCl and benzalkonium chloride in wound care solutions by HPLC J. Analytical Methods HPLC 31. J J. J Ferrer I Furlong E T. Accelerated solvent extraction 20 Kawakami S Callicott R H Zhang N. Trace analysis of mass spectrometry-mass spectrometry J. Analyst van Bruijnsvoort M Rooselaar J Stern A C Jonker K M. 22 Kovacs - Hadady K Fabian I. The determination of benzalkonium chloride in eye-drops by difference spectrophotometry J. Journal of Pharmaceutical and Biomedical Analysis Bull J P Serreqi A N Chen T Breuil C. Development of an immunoassay for a quaternary ammonium compound benzyldimethyldodecylammonium chloride J. Water Research J J J M J. 30 Shen Y Xu S J Wang S C Tu J S. Determination of benzalkonium chloride in viscous ophthalmic drops of azithromycin by high-performance liquid chromatography J. Journal of Zhejiang University Science B J

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