高效液相色谱法同时测定洗涤产品中7种防腐剂
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摘要
建立同时测定洗涤产品中4-氯-3-甲酚、双氯酚、苄氯酚、邻苯基苯酚、对氯间二甲苯酚、三氯生、三氯卡班7种防腐剂的高效液相色谱分析方法。不同基质的样品经甲醇涡旋混匀及超声提取后,用X–Bridge C18反相色谱柱(250mm×4.6 mm,5μm)进行分离,以甲醇–水为流动相,梯度洗脱,采用二极管阵列检测器(DAD)进行检测,检测波长为285 nm。在优化的实验条件下,7种防腐剂的质量浓度在0.2~500 mg/L范围内与其色谱峰面积呈良好的线性关系,相关系数(r2)均为0.999 9,方法的检出限(S/N=3)为1.0~2.5 mg/kg,定量限(S/N=10)为3.0~7.5 mg/kg。7.5,25.0,75.0 mg/kg 3水平加标回收率为92.1%~105.8%,相对标准偏差为0.8%~4.5%(n=6)。该方法简单、快速、准确,适用于洗涤产品中7种防腐剂的测定。
A method was developed for the simultaneous determination of 4-Chloro-3-cresol, dichlorophen, chlorophene, 2-phenylphenol, p-chloro-m-xylenol, triclosan and triclocarban 7 preservatives in washing products by using high performance liquid chromatography(HPLC). Samples of different types were extracted with methanol by ultrasound extraction method. Chromatographic separation was performed on a waters reversed phase column of X–Bridge C18(250 mm×4.6 mm,5 μm), with gradient elution using methanol–water as the mobile phase. The detection was performed with diode array detector(DAD). The ultraviolet detection wavelength was set at 285 nm. Under optimum conditions, the mass concentration of 7 preservatives had good linear relationship with its chromatographic peak area in the range of 0.2–500 mg/L with the same correlation coefficient(r2) of 0.999 9, the detection limits(S/N=3) for 7 preservatives were 1.0–2.5 mg/kg,and the quantification limits(S/N=10) were 3.0–7.5 mg/kg. Under three standard concentration levels of 7.5, 25.0, 75.0 mg/kg, the average recoveries of 7 preservatives were 92.1%–105.8% with the relative standard deviations of 0.8%–4.5%(n=6). The method is simple,rapid and accuracy, it is suitable for the determination of 7 preservatives in different kinds of washing products.
A method was developed for the simultaneous determination of 4-Chloro-3-cresol, dichlorophen, chlorophene, 2-phenylphenol, p-chloro-m-xylenol, triclosan and triclocarban 7 preservatives in washing products by using high performance liquid chromatography(HPLC). Samples of different types were extracted with methanol by ultrasound extraction method. Chromatographic separation was performed on a waters reversed phase column of X–Bridge C18(250 mm×4.6 mm,5 μm), with gradient elution using methanol–water as the mobile phase. The detection was performed with diode array detector(DAD). The ultraviolet detection wavelength was set at 285 nm. Under optimum conditions, the mass concentration of 7 preservatives had good linear relationship with its chromatographic peak area in the range of 0.2–500 mg/L with the same correlation coefficient(r2) of 0.999 9, the detection limits(S/N=3) for 7 preservatives were 1.0–2.5 mg/kg,and the quantification limits(S/N=10) were 3.0–7.5 mg/kg. Under three standard concentration levels of 7.5, 25.0, 75.0 mg/kg, the average recoveries of 7 preservatives were 92.1%–105.8% with the relative standard deviations of 0.8%–4.5%(n=6). The method is simple,rapid and accuracy, it is suitable for the determination of 7 preservatives in different kinds of washing products.
引文
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[17]ENNIO B,SPADARO A,SANTAGATI N A,et al.Determination of undecylenic and sorbic acids in cosmetic preparations by high performance liquid chromatography with electrochemical detection[J].Journal of pharmaceutical&biomedical analysis,2002,30(4):947–954.
[2]国家食品药品监督管理总局2015年第268号公告化妆品安全技术规范(2015)[S].
[3]ENZO S,MARIA A,AIESSANDRO B,et al.Simultaneous HPLC determination of multiple components in a commercial cosmetic cream[J].Journal of pharmaceutical&biomedical analysis,1998,18(1–2):213–217.
[4]陈德文,侯杨璐,刘宣邑,等.超声萃取高效液相色谱法测定指画颜料中的6种防腐剂[J].化学分析计量,2016,25(4):43–45.
[5]胡俊明,王骏.反相高效液相色谱法测定化妆品中防腐剂[J].色谱,2000,18(5):462–464.
[6]PHILLIPS T,BURNS A.Determination of phenols and phenates in disinfectant formulations by liquid chromatography with UV detection:collaborative study[J].Journal of aoac international,2012,95(2):411–418.
[7]OPEOLU B O,FATOKI O S,ODENDAAL J.Development of a solid-phase extraction method followed by HPLC–UV detection for the determination of phenols in water[J].International journal of physical sciences,2012,5(5):576–581.
[8]符策奕,梁颖,许文佳,等.液相色谱串联质谱法同时测定6类不同剂型化妆品中10种防腐剂[J].药物分析,2016,36(8):1 456–1 464.
[9]杨秋红,程小艳,杨坪,等.固相萃取–高效液相色谱串联质谱法同时检测地表水中的2,4-二氯酚、2,4,6-三氯酚和五氯酚[J].分析化学,2011,39(8):1 208–1 212.
[10]孙武勇,魏东伟,杨冀州,等.动物源性食品中硫氯酚残留量的高效液相色谱–电喷雾串联质谱法测定[J].分析测试学报,2009,28(10):1 213–1 216.
[11]王天娇,林勤保,宋欢,等.超高效液相色谱–串联质谱法测定食品包装纸中的酚类化合物[J].分析测试学报,2012,29(12):1 153–1 157.
[12]郑荣,茹歌,王柯.高效液相色谱–串联质谱法测定化妆品中16种防腐剂[J].中国卫生检验,2016,26(19):2 758–2 761.
[13]ROIAND B,HANS-GERHARD B,TIN W.Determination of pentachlorophenol(PCP)in waste wood—method comparison by a collaborative trial[J].Chemosphere,2002,47(9):1 001–1 006.
[14]宋春雨,王芳,王永,等.气相色谱法对化妆品中防腐剂碘丙炔基丁基氨基甲酸酯的检测[J].广东化工,2017,44(9):260–261.
[15]NICHKOVA M,GERMANI M,MARCO M P.Immunochemical analysis of 2,4,6-tribromophenol for assessment of wood contamination[J].Journal of agricultural&food chemistry,2008,56(1):29–34.
[16]LABAT L,KUMMERE E,DALLET P,et al.Comparison of high-performance liquid chromatography and capillary zone electrophoresis for the determination of parabens in a cosmetic product[J].Journal of pharmaceutical&biomedical analysis,2000,23(4):763–769.
[17]ENNIO B,SPADARO A,SANTAGATI N A,et al.Determination of undecylenic and sorbic acids in cosmetic preparations by high performance liquid chromatography with electrochemical detection[J].Journal of pharmaceutical&biomedical analysis,2002,30(4):947–954.