HPLC-MS/MS Determination of 4-Nonyl Phenol in Edible Vegetable Oils
摘 要
采用高效液相色谱-串联质谱法测定食用植物油中4-壬基酚的含量。食用植物油样品用乙酸乙酯-环己烷(1+1)混合液溶解,以凝胶渗透色谱净化,在线收集14.0~17.0 min的馏分,于30℃浓缩至近干,加甲醇1.0 mL溶解残余物。在高效液相色谱分离中,以Agilent Poroshell120ec-C18色谱柱为分离柱,以不同体积比的甲醇和0.1%(质量分数)氨水溶液的混合液为流动相进行梯度洗脱。在串联质谱分析中,采用电喷雾负离子源和多反应监测模式检测。所用内标物为4-n-NP-D4,以空白玉米油为基质。4-壬基酚的线性范围为0.25~160 μg·kg-1,方法的检出限(3S/N)为1.00 μg·kg-1。在2.00,5.00,10.00 μg·kg-1等3个浓度水平进行加标回收试验,测得回收率为99.0%~115%,测定值的相对标准偏差(n=6)为4.3%~8.1%。
Abstract
HPLC-MS/MS was applied to the determination of 4-nonyl phenol (4-NP) in edible vegetable oils. The sample of edible vegetable oil was dissolved in mixture of ethyl acetate-cyclohexane (1+1),and then purified by gel permeation chromatography, through collecting the fractions between 14.0 to 17.0 min, and the solution obtained was evaporated to near dryness at 30℃. The residue was taken up and diluted to 1.0 mL with methanol. In HPLC separation, Agilent Poroshell120ec-C18 chromatographic column was used as stationary phase, and the mixture of methanol and 0.1% (mass fraction) ammonia solution mixed in different ratios was used as mobile phase in gradient elution. In MS/MS determination, ESI- and multi-reactions monitor mode were adopted. 4-n-NP-D4 was used as internal standard and blank corn oil was used as matrix. Linearity range of 4-NP was found between 0.25 μg·kg-1 and 160 μg·kg-1 with detection limit (3S/N) of 1.00 μg·kg-1. Tests for recovery were made by standard addition method at 3 concentration levels of 2.00, 5.00, 10.00 μg·kg-1, giving values of recovery and RSD's (n=6) in the ranges of 99.0% to 115% and 4.3% to 8.1% respectively.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201805026
所属栏目 专题报道(食品分析)
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收稿日期 2017/7/24
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备注宋鑫,主管药师,研究方向为药学及理化检验,305211704@qq.com
引用该论文: SONG Xin,HANG Xueyu,WANG Qin,WANG Lu,FENG Xiaoqing. HPLC-MS/MS Determination of 4-Nonyl Phenol in Edible Vegetable Oils[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(5): 611~615
宋鑫,杭学宇,王芹,王露,冯晓青. 高效液相色谱-串联质谱法测定食用植物油中4-壬基酚的含量[J]. 理化检验-化学分册, 2018, 54(5): 611~615
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【11】俞雪钧,谷云云,冯睿,等.高效液相色谱串联质谱法同时测定海产品中双酚A及烷基酚残留[J].华中农业大学学报, 2014,33(3):52-59.
【12】赵云芝,钱蜀,谢永洪,等.固相萃取-超高效液相色谱-串联质谱法测定水中6种雌激素[J].中国环境监测, 2013,29(1):107-111.
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