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高效液相色谱-串联质谱法测定大米中高氯酸盐含量

Determination of perchlorate in rice by high performance liquid chromatography-tandem mass spectrometry
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摘要 目的建立高效液相色谱-串联质谱法测定大米中高氯酸盐的含量。方法样品提取液经过固相萃取柱快速净化处理后去除基质干扰物,采用Thermo Acclaim TRINITY P1色谱柱分离,以乙腈-20 mmol/L甲酸铵为流动相进行梯度洗脱,流速为0.3mL/min,柱温30℃,外标法定量检测。结果在高氯酸盐浓度为1.0~100.0 ng/mL的范围内的线性相关系数较好(r=0.999),检出限为4.0μg/kg,定量限为10.0μg/kg,高、中、低3个浓度水平的加标回收率在82.3%~93.2%之间,测定值的相对标准偏差小于5%(n=6)。结论该方法简便快捷、灵敏可靠,适用于大米中高氯酸盐的快速检测。 Objective To establish a method for determination of perchlorate in rice by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Methods The sample extract was quickly purified by a solid phase extraction column to remove matrix interferences.The samples were separated with a Thermo Acclaim TRINITY P1 column at the flow rate of 0.3 mL/min by gradient elute using acetonitrile and 20 mmol/L ammonium formate as mobile phase.The flow rate was 0.3 mL/min,and the column temperature was 30℃.The external standard method was used for quantitative determination.Results The linear correlation coefficient was good in the range of perchlorate concentration of 1.0 to 100.0 ng/mL(r=0.999).The limit of detection of method was 4.0μg/kg,and the limit of quantification of method was 10.0μg/kg.When the recoveries at 3 levels ranged from 82.3%to 93.2%,the values of the relation standard deviation were less than 5%(n=6).Conclusion This method is simple,rapid,sensitive and reliable,and is suitable for the rapid detection of perchlorate in rice.
作者 戴玉婷 赵琴 朱伟 曹扬 DAI Yu-Ting;ZHAO Qin;ZHU Wei;CAO Yang(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China)
出处 《食品安全质量检测学报》 CAS 2019年第7期1982-1986,共5页 Journal of Food Safety and Quality
基金 上海市科学技术委员会科研计划项目(17DZ2201200) 上海市质量技术监督局科研项目(2017-21).
关键词 高效液相色谱-串联质谱法 电喷雾离子源 大米 高氯酸盐 high performance liquid chromatography-tandem mass spectrometry electrospray ionization rice perchlorate
作者简介 戴玉婷,硕士,工程师,主要研究方向为食品安全检测。E-mail:daiyt@sqi.org.cn;通讯作者:赵琴,工程师,主要研究方向为食品安全检测。E-mail:zhaoqin@sqi.org.cn
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