气相色谱-质谱法测定皮革中对苯二胺含量
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摘要
采用气相色谱一质谱法测定皮革中的对苯二胺含量。通过对色谱参数、提取方式、提取温度、提取时间、提取次数等条件的优化,建立了皮革中对苯二胺含量的检测方法。对苯二胺标准曲线线性范围为0.1～5.0 mg/L,相关系数为0.9996,检出限为1.22 mg/kg,平均回收率为86.4%～108.2%,相对标准偏差(RSDs,n=6)为3.52%～7.48%。
P-phenylenediamine in leather was analyzed by gas chromatography-mass spectrometry(GC-MS). The experi?mental conditions were optimized including chromatography parameter,extraction method,extraction temperature,extrac?tion time and extraction times. The results demonstrated that the standard curve linear range of p-phenylenediamine was 0.1～5.0 mg/L,the correlation coeficient was 0.9996 and the detection limit was 1.22 mg/kg. The average recoveries of pphenylenediamine were in the range of 86.4% ～108.2%,and the relative standard deviations(RSDs,n=6)were 3.52%～7.48%.
P-phenylenediamine in leather was analyzed by gas chromatography-mass spectrometry(GC-MS). The experi?mental conditions were optimized including chromatography parameter,extraction method,extraction temperature,extrac?tion time and extraction times. The results demonstrated that the standard curve linear range of p-phenylenediamine was 0.1～5.0 mg/L,the correlation coeficient was 0.9996 and the detection limit was 1.22 mg/kg. The average recoveries of pphenylenediamine were in the range of 86.4% ～108.2%,and the relative standard deviations(RSDs,n=6)were 3.52%～7.48%.
引文
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[3]ISO/TR 16178:2012 Footwear-Critical substances potentially present in footwear and footwear components[S].
[4]GB/T 24800.12-2009化妆品中对苯二胺、邻苯二胺和间苯二胺的测定[S].
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[9]胡望霞,林紫威,洪杰,等.气相色谱-质谱法测定鞋材中的对苯二胺[J].皮革与化工,2017,36(4):12-14.
[10]康瑞琴,苏文辉,张鑫,等.高效液相色谱法测定染发剂中对苯二胺的含量[J].化学工程师,2015,235(4):23-25.
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[12]郭雅妮,任伟琴,郁翠华,等.纺织品4-氨基偶氮苯检测方法的试验研究[J].棉纺织技术,2010,38(8):29-31.
[13]赵嵩,张菁.出口纺织品中禁用的4一氨基偶氮苯检测方法探讨[J].上海丝绸,2007,3:2-13.
[2]熊杰,钱蜀,李海霞,等.超高效液相色谱一串联四极杆质谱分析环境水样中对苯二胺[J].四川环境,2013,32(3):24-27.
[3]ISO/TR 16178:2012 Footwear-Critical substances potentially present in footwear and footwear components[S].
[4]GB/T 24800.12-2009化妆品中对苯二胺、邻苯二胺和间苯二胺的测定[S].
[5]袁慧,浦跃朴,尹立红,等.对苯二胺氧化产物对小鼠经皮肤染毒的亚慢性毒性[J].环境与职业医学,2002,19(5):290-292.
[6]谢碧俊,杨长晓.毛细管气相色谱测定工作场所空气中对苯二胺[J].预防医学情报杂志,2011,11:952-955.
[7]曹美龄,徐立,麦琦.染发剂中对苯二胺的测定方法研究与改进[J].中国卫生检验杂志,2008,18(1):168-169.
[8]吴新,谭朝勤.氧化型染发剂中对苯二胺的气液相色谱分析方法比较[J].广东化工,2009,36(8):207-208.
[9]胡望霞,林紫威,洪杰,等.气相色谱-质谱法测定鞋材中的对苯二胺[J].皮革与化工,2017,36(4):12-14.
[10]康瑞琴,苏文辉,张鑫,等.高效液相色谱法测定染发剂中对苯二胺的含量[J].化学工程师,2015,235(4):23-25.
[11]苗力孝,马红艳,孙雪花,等.方波溶出伏安法快速测定染发剂中对苯二胺[J].延安大学学报,2008,27(3):71-74.
[12]郭雅妮,任伟琴,郁翠华,等.纺织品4-氨基偶氮苯检测方法的试验研究[J].棉纺织技术,2010,38(8):29-31.
[13]赵嵩,张菁.出口纺织品中禁用的4一氨基偶氮苯检测方法探讨[J].上海丝绸,2007,3:2-13.