固相萃取-高效液相色谱法测定纸质食品包装材料中五氯酚含量  

Determination of pentachlorophenol by solid phase extraction-high performance liquid chromatography in paper packaging materials for foodstuffs

作　　者：陆阳 朱鹏飞[1] 姚誉阳[1] 潘春燕 邵彪 吴宇伉 LU YANG;ZHU Peng-Fei;YAO Yu-Yang;PAN Chun-Yan;SHAO Biao;WU Yu-Kang(Wuxi Centre for Disease Control and Prevention,Jiangsu Provincial Key Laboratory of Food Safety Risk Monitoring(In the field of Organic Pollutants)Wuxi 214023,China;Nantong Products Quality Supervision and Inspection,Nantong 220611,China)

机构地区：[1]无锡市疾病预防控制中心,江苏省食品安全风险监测重点实验室(有机污染物领域),无锡214023 [2]南通市产品质量监督检验所,南通220611

出　　处：《食品安全质量检测学报》2022年第1期65-71,共7页Journal of Food Safety and Quality

基　　金：无锡市“科教强卫工程”项目[CXPT(SYS)002];“双百”卫生人才-后备拔尖人才-朱鹏飞项目。

摘　　要：目的建立固相萃取-高效液相色谱法测定纸质食品包装材料中五氯酚的分析方法。方法2 g样品经过0.5%甲酸-甲醇超声提取2次,合并提取液,经Waters Oasis PRiME HLB(200 mg/6 mL)固相萃取小柱净化,洗脱液氮吹浓缩至近干,经甲醇复溶后采用高效液相色谱-二极管阵列检测器测定,以C_(18)柱为色谱柱,甲醇-5 mmol/L乙酸铵(65:35,V:V)为流动相,等度洗脱,流速为1.0 mL/min,柱温为35℃,进样量为20μL,检测波长为217 nm。结果五氯酚在0.05~10.00μg/mL范围内线性关系良好,相关系数大于0.999,检出限为0.01 mg/kg,定量限为0.03 mg/kg,平均加标回收率为84.7%~92.8%,相对标准偏差(relative standard deviations,RSDs)为1.74%~4.79%。结论该方法回收率高、重复性好、前处理简便,可用于纸质食品包装材料中五氯酚的大批量检测。Objective To establish an analytical method for the determination of pentachlorophenol in paper packaging materials for foodstuffs by solid phase extraction-high performance liquid chromatography.Methods The 2 g samples were ultrasonically extracted with 0.5%formic acid and methanol twice,the extracted solution was combined,and purified by Waters Oasis PRiME HLB(200 mg/6 mL)solid phase extraction cartridge,the eluent was concentrated by blowing nitrogen to near dryness,then redissolved in methanol,and determined by high performance liquid chromatography-diode array detector.The separation was performed on C_(18) column using methanol-5 mmol/L ammonium acetate(65:35,V:V)as mobile phase for isocratic elution.The flow rate was 1.0 mL/min,column temperature was 35℃,sample size was 20μL,and the detection wavelength was 217 nm.Results Pentachlorophenol had a good linear relationship in the range of 0.05-10.00μg/mL,the correlation coefficient was greater than 0.999,the limit of detection was 0.01 mg/kg,the limit of quantification was 0.03 mg/kg,and the average recoveries were 84.7%-92.8%,the relative standard deviations were 1.74%-4.79%.Conclusion The method has high recovery,good repeatability,simple pre-treatment,and can be used for large-scale detection of pentachlorophenol in paper packaging materials for foodstuffs.

关 键 词：固相萃取 高效液相色谱法 纸质食品包装材料 五氯酚 

分 类 号：O657.72[理学—分析化学] TS206.4[理学—化学]