食用槟榔中多种对羟基苯甲酸酯类残留量的测定与确证
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摘要
为建立食用槟榔中对羟基苯甲酸甲酯、对羟基苯甲酸乙酯、对羟基苯甲酸丙酯和对羟基苯甲酸丁酯残留量的气相色谱检测和气质联用确证的方法,用乙醚萃取经盐酸酸化后的提取液,分别用饱和氯化钠溶液和碳酸氢钠溶液对乙醚层进行洗涤后浓缩,氮吹至近干后用乙醇定容。采用DB-5毛细管柱(30 m×0.32 mm×0.25μm)进行仪器分析。气相色谱法在4～200μg/m L质量浓度范围内线性良好, r~2均大于0.999 5,分别对2.0, 5.0和20.0μg/m L进行加标回收试验,回收率在83.6%～103.6%之间, 4种对羟基苯甲酸酯类的定量下限均为0.1 mg/kg,标准物质分离度在10.0以上。气质联用法采用SIM扫描,在2～10μg/m L质量浓度范围r2均大于0.998, 4种对羟基苯甲酸酯类的定量下限分别为0.012, 0.01, 0.01和0.01 mg/kg。气质联用法能有效地将二丁基羟基甲苯(BHT)与对羟基苯甲酸乙酯分开,避免假阳性的出现。该方法适用于槟榔等复杂基质样品中对羟基苯甲酸酯类物质的检测。
A method for the determination of methyl para hydroxybenzoate, ethyl para hydroxy benzoate, propyl para hydroxy benzoate and butyl para hydroxy benzoate in areca was established by gas chromatography and GC-MS. After acidification with hydrochloric acid, the ether layer was washed with saturated sodium chloride solution and sodium bicarbonate solution.DB-5 capillary column(30 m×0.32 mm, 0.25 μm) was adopted for GC. By GC method, the correlation coefficients were greater than 0.999 5 in the range of 4-200 μg/mL. The recoveries of 2, 5 and 20 μg/mL were determined between 83.5% and103.6%. The lower limits of quantitation of all the 4 kinds of hydroxyl benzoic acid esters were 0.1 mg/kg, and the separation degree of standard material was more than 10.0. By GC-MS, the correlation coefficients were greater than 0.998 in the range of 2-10 μg/mL. The lower limits of quantitation of the 4 kinds of hydroxyl benzoic acid esters were 0.012, 0.1, 0.1, and 0.1 mg/kg, respectively. Gas chromatography-mass spectrometry could effectively distinguish dibutyl hydroxy toluene(BHT) and ethyl p-hydroxybenzoate, which can avoid the occurrence of false positives. This method was suitable for the detection of parabens in areca nut.
A method for the determination of methyl para hydroxybenzoate, ethyl para hydroxy benzoate, propyl para hydroxy benzoate and butyl para hydroxy benzoate in areca was established by gas chromatography and GC-MS. After acidification with hydrochloric acid, the ether layer was washed with saturated sodium chloride solution and sodium bicarbonate solution.DB-5 capillary column(30 m×0.32 mm, 0.25 μm) was adopted for GC. By GC method, the correlation coefficients were greater than 0.999 5 in the range of 4-200 μg/mL. The recoveries of 2, 5 and 20 μg/mL were determined between 83.5% and103.6%. The lower limits of quantitation of all the 4 kinds of hydroxyl benzoic acid esters were 0.1 mg/kg, and the separation degree of standard material was more than 10.0. By GC-MS, the correlation coefficients were greater than 0.998 in the range of 2-10 μg/mL. The lower limits of quantitation of the 4 kinds of hydroxyl benzoic acid esters were 0.012, 0.1, 0.1, and 0.1 mg/kg, respectively. Gas chromatography-mass spectrometry could effectively distinguish dibutyl hydroxy toluene(BHT) and ethyl p-hydroxybenzoate, which can avoid the occurrence of false positives. This method was suitable for the detection of parabens in areca nut.
引文
[1]中华人民共和国国家卫生和计划生育委员会.食品安全国家标准食品添加剂使用标准:GB 2760-2014[S].北京:中国标准出版社,2014.
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[3]海南省质量技术监督局.食用槟榔:DB 46/T 75-2007[S].2007.
[4]中华人民共和国国家卫生和计划生育委员会.食品中对羟基苯甲酸酯类的测定:GB/T 5009.31-2016[S].北京:中国标准出版社,2016.
[5]杨卫花,赵浩军,杨慰,等.毛细管气相色谱法测定酱腌菜中的对羟基苯甲酸酯类的含量[J].云南化工,2011,38(5):31-33.
[6]陈幸莺.食品中12种防腐剂多通量测定方法的研究[J].食品与机械,2015,31(2):134-139.
[7]谢敢爱,何浩.槟榔中对羟基苯甲酸酯类的快速测定-气相色谱法[J].商品与质量,2012(12):262.
[8]山东省质量技术监督局.食品中对羟基苯甲酸酯类的测定高效液相色谱法:DB 37/T 1100-2008[S].2008.
[9]食品中对羟基苯甲酸酯类的测定高效液相色谱法:DBS53/014-2013[S].2014.
[10]刘佟,王浩,苗雨田,等.高效液相色谱法同时测定食品中种防腐剂[J].食品安全质量检测学报,2015,6(4):1148-1153.
[11]陈沛金,张毅,肖锋,等.高效液相色谱法测定糖果、蜜饯、饮料中19种食品添加剂[J].食品安全质量检测学报,2014,5(11):3487-3494.
[12]鞠福龙,李东时,李春娟.GC-MS-SIM法同时分析饮料中防腐剂和抗氧化剂[J].现代科学仪器,2010(1):77-79.
[13]李春娟,鞠福龙,李东时.GC-MS法同时检测葡萄酒中10种防腐剂和抗氧化剂[J].中国酿造,2009(6):149-152.
[14]郝鹏飞,徐琴,牟志春,等.气相色谱-质谱法同时测定葡萄酒中13种防腐剂[J].分析实验室,2013,32(7):108-112.
[15]ROUTLEDGE E J,PARKER J,ODUM J,et al.Some alkyl hydroxy benzoate preservatives(parabens)are estrogenic[J].Toxicol Appl Pharmacol,1998,153(1):12-19.
[16]OISHI S.Effects of butylparaben on the reproductive system in rats[J].Toxicol Ind Health,2001,17(1):31-39.
[17]OISHI S.Effects of propyl paraben on the male reproductive system[J].Food Chem Toxicol,2002,40(12):1807-1813.
[2]湖南省质量技术监督局.食用槟榔:DB 43/132-2004[S].2004.
[3]海南省质量技术监督局.食用槟榔:DB 46/T 75-2007[S].2007.
[4]中华人民共和国国家卫生和计划生育委员会.食品中对羟基苯甲酸酯类的测定:GB/T 5009.31-2016[S].北京:中国标准出版社,2016.
[5]杨卫花,赵浩军,杨慰,等.毛细管气相色谱法测定酱腌菜中的对羟基苯甲酸酯类的含量[J].云南化工,2011,38(5):31-33.
[6]陈幸莺.食品中12种防腐剂多通量测定方法的研究[J].食品与机械,2015,31(2):134-139.
[7]谢敢爱,何浩.槟榔中对羟基苯甲酸酯类的快速测定-气相色谱法[J].商品与质量,2012(12):262.
[8]山东省质量技术监督局.食品中对羟基苯甲酸酯类的测定高效液相色谱法:DB 37/T 1100-2008[S].2008.
[9]食品中对羟基苯甲酸酯类的测定高效液相色谱法:DBS53/014-2013[S].2014.
[10]刘佟,王浩,苗雨田,等.高效液相色谱法同时测定食品中种防腐剂[J].食品安全质量检测学报,2015,6(4):1148-1153.
[11]陈沛金,张毅,肖锋,等.高效液相色谱法测定糖果、蜜饯、饮料中19种食品添加剂[J].食品安全质量检测学报,2014,5(11):3487-3494.
[12]鞠福龙,李东时,李春娟.GC-MS-SIM法同时分析饮料中防腐剂和抗氧化剂[J].现代科学仪器,2010(1):77-79.
[13]李春娟,鞠福龙,李东时.GC-MS法同时检测葡萄酒中10种防腐剂和抗氧化剂[J].中国酿造,2009(6):149-152.
[14]郝鹏飞,徐琴,牟志春,等.气相色谱-质谱法同时测定葡萄酒中13种防腐剂[J].分析实验室,2013,32(7):108-112.
[15]ROUTLEDGE E J,PARKER J,ODUM J,et al.Some alkyl hydroxy benzoate preservatives(parabens)are estrogenic[J].Toxicol Appl Pharmacol,1998,153(1):12-19.
[16]OISHI S.Effects of butylparaben on the reproductive system in rats[J].Toxicol Ind Health,2001,17(1):31-39.
[17]OISHI S.Effects of propyl paraben on the male reproductive system[J].Food Chem Toxicol,2002,40(12):1807-1813.