Determination of Benzalkonium Bromide and o-Phthalaldehyde in Quaternary Ammonium Salt Compound Disinfectant by HPLC
摘 要
建立了高效液相色谱法(HPLC)同时测定季铵盐复合消毒液样品中苯扎溴铵和邻苯二甲醛(OPA)含量的方法。用流动相[体积比为1∶1的0.02 mol·L-1的乙酸-乙酸铵缓冲溶液(pH 4.5)和甲醇混合而成]将1.0 mL样品定容至10.0 mL,涡旋混合5 min后过0.45 μm滤膜,取滤液供HPLC分析。以XDB-C18色谱柱为固定相,用流动相进行等度洗脱分离,在检测波长263 nm处测定目标物。结果表明,苯扎溴铵和OPA标准曲线的线性范围均为10.0~800.0 mg·L-1,方法检出限(3S/N)分别为5.0,3.5 mg·L-1。以此方法分析了3个样品,所得结果和标示值一致,测定值的相对标准偏差(n=7)均小于1.0%。以这3个样品为基质进行3个浓度水平的加标回收试验,得到苯扎溴铵和OPA的回收率分别为93.7%~95.2%和94.5%~98.5%。
Abstract
A HPLC method for simultaneous determination of benzalkonium bromide and o-phthalaldehyde (OPA) in quaternary ammonium compound salt disinfectant was established. 1.0 mL of the sample was made up to 10.0 mL with the mobile phase[mixture composed of 0.02 mol·L-1 acetic acid-ammonium acetate buffer solution (pH 4.5) and methanol in the volume ratio of 1:1] as dilution solvent. After mixing for 5 minutes by votex, the sample solution was passed through a 0.45 μm filter membrane, and the 2 analytes in the filtrate were determined by HPLC at the detection wavelength of 263 nm under conditions using XDB-C18 column as stationary phase and isocratic elution with mobile phase. As found by results that linearity range of standard curves of benzalkonium bromide and OPA was found same in the range of 10.0-800.0 mg·L-1, and detection limits of benzalkonium bromide and OPA were 5.0, 3.5 mg·L-1, respectively. The 3 sample were analyzed by the above method, and results obtained were in conformity with the label values, with RSDs (n=7) of determined values lower than 1.0%. Recovery test was made by standard addition method using the 3 samples as matrixes at the 3 concentration levels, giving values of recovery of 93.7%-95.2% and 94.5%-98.5%, respectively.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202011011
所属栏目 工作简报
基金项目 河南省青年骨干教师项目(2018GGJS278);河南省科技攻关项目(182102310283);河南省高等学校重点项目(19A330001)
收稿日期 2020/4/9
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备注睢超霞,副教授,硕士,主要从事医学化学的科研与教学工作,suichaoxia@1foxmail.com
引用该论文: SUI Chaoxia,WANG Shuyu,WANG Ke. Determination of Benzalkonium Bromide and o-Phthalaldehyde in Quaternary Ammonium Salt Compound Disinfectant by HPLC[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2020, 56(11): 1201~1204
睢超霞,王舒雨,王克. 高效液相色谱测定季铵盐复合消毒液中的苯扎溴铵和邻苯二甲醛[J]. 理化检验-化学分册, 2020, 56(11): 1201~1204
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【3】林立旺,许能锋,陈菁,等.复方邻苯二甲醛的研制及消毒性能观察[J].中国消毒学杂志, 2007,24(1):21-25.
【4】董小峰,蒋丽娟,张晓玲,等.邻苯二甲醛与苯扎溴铵协同杀菌作用研究[J].中国消毒学杂志, 2019,36(4):244-245.
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【8】OH J A, SHIN H S. Determination of ortho-phthalaldehyde in water by high performance liquid chromatography and gas chromatography-mass spectrometry after hydrazine derivatization[J]. Journal of Chromatography A, 2012,1247:99-103.
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【12】甘露.离子对高效液相色谱法检测滴眼液中苯扎溴铵含量[J].黑龙江医药, 2011,24(5):695-696.
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