高效液相色谱法同时测定婴儿湿巾中9种防腐剂
|
摘要
称取0.500 0g湿巾样品,剪碎后,加入80%(体积分数)甲醇溶液5.00mL,漩涡振荡提取3min,经0.22μm滤膜过滤,以Diamonsil C_(18)(2)色谱柱(4.6mm×250mm,5μm)分离滤液中的9种防腐剂,流动相为甲醇-0.1%(质量分数)磷酸溶液,梯度洗脱。采用二极管阵列检测器,咪唑烷基脲、5,5-二甲基海因、2-溴-2-硝基丙烷-1,3-二醇、苄索氯胺和苯扎氯铵的检测波长为210nm,氯苯酣醚的检测波长为230nm,醋酸氯己定、山梨酸钾和氯化十六烷基吡啶的检测波长为254nm。9种防腐剂的质量浓度在一定范围内与对应的色谱峰面积呈线性关系,检出限(3S/N)在0.01～0.5mg·L~(-1)之间。对空白样品进行加标回收试验,回收率在77.2%～100%之间,测定值的相对标准偏差(n=6)在1.2%～8.4%之间。应用该方法分析了20批次婴儿湿巾样品,有15批次的样品中检出咪唑烷基脲、5,5-二甲基海因、2-溴-2-硝基丙烷-1,3-二醇、醋酸氯己定、山梨酸钾或苄索氯胺。
The wipe sample(0.500 0 g) was cut and extracted with 5.00 mL of 80%(volume fraction) methanol solution by vortex oscillation for 3 min.After filtrating through 0.22μm filter membrane,9 preservatives in the filtrate were separated on a Diamonsil C_(18)(2) column(4.6 mm×250 mm,5μm),with a mixture of methanol and 0.1%(mass fraction) phosphoric acid solution as mobile phase for gradient elution,and detected by a diode array detector,at the wavelength of 210 nm for imidazolidinyl urea,5,5-dimethylhydantoin,2-bromo-2-nitropropane-1,3-diol,benzethonamide and benzalkonium chloride,230 nm for chlorobenzoate,254 nm for chlorhexidine acetate,potassium sorbate and cetylpyridinium chloride.Linear relationships were found between chromatographic area peak and mass concentration of 9 preservatives in definite ranges,with detection limits(3 S/N) in the range of 0.01-0.5 mg·L~(-1).Test for recovery was made by standard addition method on the base of blank sample,giving results in the range of 77.2%-100%,with the relative standard deviations(RSDs,n=6) ranged from 1.2% to 8.4%.The proposed method was used to analyze 20 batches of baby wet wipes,and imidazolidinyl urea,5,5-dimethylhydantoin,2-bromo-2-nitropropane-1,3-diol,chlorhexidine acetate,potassium sorbate,benzethonamide were found in 15 batches of samples.
The wipe sample(0.500 0 g) was cut and extracted with 5.00 mL of 80%(volume fraction) methanol solution by vortex oscillation for 3 min.After filtrating through 0.22μm filter membrane,9 preservatives in the filtrate were separated on a Diamonsil C_(18)(2) column(4.6 mm×250 mm,5μm),with a mixture of methanol and 0.1%(mass fraction) phosphoric acid solution as mobile phase for gradient elution,and detected by a diode array detector,at the wavelength of 210 nm for imidazolidinyl urea,5,5-dimethylhydantoin,2-bromo-2-nitropropane-1,3-diol,benzethonamide and benzalkonium chloride,230 nm for chlorobenzoate,254 nm for chlorhexidine acetate,potassium sorbate and cetylpyridinium chloride.Linear relationships were found between chromatographic area peak and mass concentration of 9 preservatives in definite ranges,with detection limits(3 S/N) in the range of 0.01-0.5 mg·L~(-1).Test for recovery was made by standard addition method on the base of blank sample,giving results in the range of 77.2%-100%,with the relative standard deviations(RSDs,n=6) ranged from 1.2% to 8.4%.The proposed method was used to analyze 20 batches of baby wet wipes,and imidazolidinyl urea,5,5-dimethylhydantoin,2-bromo-2-nitropropane-1,3-diol,chlorhexidine acetate,potassium sorbate,benzethonamide were found in 15 batches of samples.
引文
[1] 张训岭.中国湿巾市场潜力巨大婴儿湿巾将首先实现突破[J].生活用纸,2014(16):24-26.
[2] GB/T 27728-2011 湿巾[S].
[3] GB 15979-2002 一次性使用卫生用品卫生标准[S].
[4] 王海涛,何聪芬,董银卯.化妆品接触性皮炎的发病机理探究[J].香料香精化妆品,2008(5):23-26.
[5] 韩玉杰,戚士龙,唐镇忠,等.自动电位滴定仪测定硼化物方法[J].中国木材,2014(5):35-37.
[6] 裘曦,杨云霞.分光光度法在食品防腐剂检测中的运用探讨[J].食品安全导刊,2016(12):114-114.
[7] 赵娅鸿.气相色谱法测定食品中防腐剂单辛酸甘油酯[J].理化检验-化学分册,2011,47(11):1354-1356.
[8] 刘晓慧,刘谦,吴新欣,等.高效液相色谱法测定不同基质的食品中防腐剂含量[J].理化检验-化学分册,2017,53(4):447-450.
[9] 王改香,张磊,唐晓军,等.气相色谱-质谱法测定化妆品中10种防腐剂[J].理化检验-化学分册,2015,51(1):35-38.
[10] 凌云,储晓刚,张峰,等.超高效液相色谱-串联质谱法同时测定调味料中的17种防腐剂和抗氧化剂[J].色谱,2011,29(8):723-730.
[11] TZANAVARAS P D,KARAKOSTA T D,RIGAS P G,et al.Isocratic liquid chromatographic determination of three paraben preservatives in hygiene wipes using a reversed phase core-shell narrow-bore column[J].Central European Journal of Chemistry,2012,10(5):1459-1463.
[12] CELEIRO M,LAMAS J P,GARCIA-JARES C,et al.Pressurized liquid extraction-gas chromatographymass spectrometry analysis of fragrance allergens,musks,phthalates and preservatives in baby wipes[J].Journal of Chromatography A,2015,1384(6):9-21.
[13] 龚越飞,金训伦,周江.超高效液相色谱带PDA检测器法快速测定湿巾中9种防腐剂[J].中国卫生检验杂志,2017(8):1084-1087.
[14] 龚越飞,周江,金训伦.超高效液相色谱法测定湿巾中7种防腐剂[J].化学分析计量,2017,26(2):57-60.
[15] 郑芸芸,李琼,张健.化妆品中限用防腐剂咪唑烷基脲和DMDM乙内酰脲的检测方法综述[J].应用技术学报,2011,11(1):7-11.
[16] 王萍,李洁,郑和辉.超高效液相色谱法测定化妆品中22种防腐剂[J].中国卫生检验杂志,2009,19(6):1291-1293.
[17] 陈彦凤,李俐,孙艳芳,等.反相高效液相色谱法测定消毒产品中葡萄糖酸氯己定含量[J].中国卫生检验杂志,2017(14):2000-2001.
[18] 张泽生,吴天宸,郭擎,等.食品中苯甲酸和山梨酸检测样品前处理方法研究进展[J].中国食品添加剂,2015(5):162-167.
[19] 朱会卷,张卫强,杨艳伟,等.高效液相色谱分析化妆品中的防腐剂氯苯甘醚[J].色谱,2014,32(1):95-99.
[20] 刘艳琴,王浩,杨红梅,等.高效液相色谱法同时测定化妆品中的3种苯扎氯铵同系物[J].色谱,2011,29(5):458-461.
[21] 左家信,曾栋,李帮锐,等.高效液相色谱法测定消毒液中的苯扎氯铵和苯扎溴铵[J].中国卫生检验杂志,2017(12):1688-1692.
[22] 丁宏,张鹏祥,高晓譞,等.HPLC法测定化妆品中防腐剂劳拉氯铵、苄索氯铵和西他氯铵的含量[J].中国药事,2012,26(8):830-833.
[2] GB/T 27728-2011 湿巾[S].
[3] GB 15979-2002 一次性使用卫生用品卫生标准[S].
[4] 王海涛,何聪芬,董银卯.化妆品接触性皮炎的发病机理探究[J].香料香精化妆品,2008(5):23-26.
[5] 韩玉杰,戚士龙,唐镇忠,等.自动电位滴定仪测定硼化物方法[J].中国木材,2014(5):35-37.
[6] 裘曦,杨云霞.分光光度法在食品防腐剂检测中的运用探讨[J].食品安全导刊,2016(12):114-114.
[7] 赵娅鸿.气相色谱法测定食品中防腐剂单辛酸甘油酯[J].理化检验-化学分册,2011,47(11):1354-1356.
[8] 刘晓慧,刘谦,吴新欣,等.高效液相色谱法测定不同基质的食品中防腐剂含量[J].理化检验-化学分册,2017,53(4):447-450.
[9] 王改香,张磊,唐晓军,等.气相色谱-质谱法测定化妆品中10种防腐剂[J].理化检验-化学分册,2015,51(1):35-38.
[10] 凌云,储晓刚,张峰,等.超高效液相色谱-串联质谱法同时测定调味料中的17种防腐剂和抗氧化剂[J].色谱,2011,29(8):723-730.
[11] TZANAVARAS P D,KARAKOSTA T D,RIGAS P G,et al.Isocratic liquid chromatographic determination of three paraben preservatives in hygiene wipes using a reversed phase core-shell narrow-bore column[J].Central European Journal of Chemistry,2012,10(5):1459-1463.
[12] CELEIRO M,LAMAS J P,GARCIA-JARES C,et al.Pressurized liquid extraction-gas chromatographymass spectrometry analysis of fragrance allergens,musks,phthalates and preservatives in baby wipes[J].Journal of Chromatography A,2015,1384(6):9-21.
[13] 龚越飞,金训伦,周江.超高效液相色谱带PDA检测器法快速测定湿巾中9种防腐剂[J].中国卫生检验杂志,2017(8):1084-1087.
[14] 龚越飞,周江,金训伦.超高效液相色谱法测定湿巾中7种防腐剂[J].化学分析计量,2017,26(2):57-60.
[15] 郑芸芸,李琼,张健.化妆品中限用防腐剂咪唑烷基脲和DMDM乙内酰脲的检测方法综述[J].应用技术学报,2011,11(1):7-11.
[16] 王萍,李洁,郑和辉.超高效液相色谱法测定化妆品中22种防腐剂[J].中国卫生检验杂志,2009,19(6):1291-1293.
[17] 陈彦凤,李俐,孙艳芳,等.反相高效液相色谱法测定消毒产品中葡萄糖酸氯己定含量[J].中国卫生检验杂志,2017(14):2000-2001.
[18] 张泽生,吴天宸,郭擎,等.食品中苯甲酸和山梨酸检测样品前处理方法研究进展[J].中国食品添加剂,2015(5):162-167.
[19] 朱会卷,张卫强,杨艳伟,等.高效液相色谱分析化妆品中的防腐剂氯苯甘醚[J].色谱,2014,32(1):95-99.
[20] 刘艳琴,王浩,杨红梅,等.高效液相色谱法同时测定化妆品中的3种苯扎氯铵同系物[J].色谱,2011,29(5):458-461.
[21] 左家信,曾栋,李帮锐,等.高效液相色谱法测定消毒液中的苯扎氯铵和苯扎溴铵[J].中国卫生检验杂志,2017(12):1688-1692.
[22] 丁宏,张鹏祥,高晓譞,等.HPLC法测定化妆品中防腐剂劳拉氯铵、苄索氯铵和西他氯铵的含量[J].中国药事,2012,26(8):830-833.