Cleaning validation 1: development and validation of a chromatographic method for the detection of traces of LpHse detergent.
Cleaning validation 1: development and validation of a chromatographic method for the detection of traces of LpHse detergent.
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清洁验证 1：开发和验证用于检测痕量 LpHse 清洁剂的色谱方法。
DOI：
10.1016/j.jpba.2005.10.049
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发表时间：
2006
影响因子：
3.4
通讯作者：
Leyda M Ramos
中科院分区：
文献类型：
--
作者：
J. Zayas;Héctor Colón;Omar Garced;Leyda M Ramos
建立了一种高效液相色谱法（HPLC）检测痕量LpHse（4-叔戊基苯酚和2-苯基苯酚）的方法。该方法在溶液中0.5 - 10.00 ppm范围内呈线性。该方法也被证明是准确的，通过拭子材料从金属表面（4″×4″未抛光的304不锈钢板）的戊基苯酚的面积响应回收率高达95%，苯基苯酚的面积响应回收率高达94%。该方法的重现性测定为1.61%（戊基苯酚的峰面积响应值和峰高响应值）和1.52%（苯基苯酚的峰面积响应值和峰高响应值），报告为合并相对标准偏差。通过比较不同分析员的不同制备物，也表明所开发的方法具有耐用性。溶液中戊基苯酚的检测限确定为0.076 ppm（峰面积）、0.079 ppm（峰高度），苯基苯酚的检测限确定为0.34 ppm（峰面积）、0.82 ppm（峰高度），金属研究回收率中戊基苯酚的检测限确定为1.77 ppb（峰面积）、1.23 ppm（峰高度），苯基苯酚的检测限确定为1.23 ppm（峰面积）、1.44 ppm（峰高度）。溶液中戊基苯酚的定量限确定为0.25 ppm（峰面积）、0.26 ppm（峰高度），苯基苯酚的定量限确定为1.14 ppm（峰面积）、2.73 ppm（峰高度），金属板回收率研究中戊基苯酚的定量限确定为3.89 ppm（峰面积）、4.11 ppm（峰高度），苯基苯酚的定量限确定为4.11 ppm（峰面积）、4.79 ppm（峰高度）。该方法可用于测定使用清洁剂的清洁设备中是否存在LpHse残留物。
A high performance liquid chromatography (HPLC) method for the detection of traces of LpHse (4-tert-amylphenol and 2-phenylphenol) has been developed and validated. The method was shown to be linear in the range from 0.5 to 10.00ppm in solution. The method was also shown to be accurate with a recovery of up to 95% by area response for amylphenol and up to 94% by area response for phenylphenol from metal surfaces (4″×4″ un-polished 304 stainless steel plates) by means of swab material. The reproducibility of the method was determined to be 1.61% by area response and 1.52% by height response for amylphenol and 5.40% by area response and 13.77% by height response for phenylphenol from solutions reported as the pooled relative standard deviation. The developed method was also shown to be rugged by comparisons of different preparations by different analysts. The limit of detection was established to be 0.076ppm by peak area, 0.079ppm by peak height for amylphenol and 0.34ppm by peak area, 0.82ppm by peak height for phenylphenol from solution, and 1.77ppb by peak area, 1.23ppm by peak height for amylphenol and 1.23ppm by peak area, 1.44ppm by peak height for phenylphenol from recovery from metal studies. The limit of quantitation was established to be 0.25ppm by peak area, 0.26ppm by peak height for amylphenol and 1.14ppm by peak area, 2.73ppm by peak height for phenylphenol from solution, and 3.89ppm by peak area, 4.11ppm by peak height for amylphenol and 4.11ppm by peak area, 4.79ppm by peak height for phenylphenol from recovery from metal plates studies. This method can be employed to determine the presence of LpHse residues in cleaned equipments where the detergent was used.