土壤中氯硝柳胺残留的超高效液相色谱-串联质谱测定法  

Determination of niclosamide residue in soil by ultra performance liquid chromatography tandem mass spectrometry

作　　者：和佳鸳 王琳[1] 潘春燕[1] 徐虹[1] 易承学 HE Jia-yuan;WANG Lin;PAN Chun-yan;XU Hong;YI Cheng-xue(Physical and Chemical Laboratory,Zhenjiang Center for Disease Control and Prevention,Zhenjiang Jumgsu,212004,China;School of Pharmaceutical Technology,Zhenjiang College,Zlienjicing Jiangsu,212028,China)

机构地区：[1]镇江市疾病预防控制中心检验科,江苏镇江212004 [2]镇江市高等专科学校医药技术学院,江苏镇江212028

出　　处：《职业与健康》2021年第4期472-475,共4页Occupation and Health

基　　金：江苏省血地寄防科研课题(X201801);江苏省“科教强卫工程”专项经费资助(QNRC2016461);镇江市高等专科学校高层次人才科研启动基金(2037080062)。

摘　　要：目的建立测定土壤中氯硝柳胺残留的超高效液相色谱串联质谱(UHPLC-MS/MS)方法。方法土壤样品经乙腈超声提取、高速离心后,取上清液过滤后采用UHPLC-MS/MS测定,外标法定量。以Waters BEH C18色谱柱为固定相,以不同体积比的甲醇和水的混合液为流动相进行梯度洗脱,串联质谱中采用电喷雾负离子源和多反应监测模式。结果氯硝柳胺的质量浓度在0.002~0.080 mg/L内与其对应的峰面积成线性关系(r=0.999 6),方法的检出限为5×10^(-4) ng,定量限(LOQ)为0.5μg/kg;在0.02、0.10、0.20 mg/kg 3个添加水平下,平均回收率为73.4%~79.8%,相对标准偏差(RSD)为1.5%~3.3%。结论该方法简单、高效、灵敏度高、准确性好,适用于土壤中氯硝柳胺的测定。Objective To establish an ultra performance liquid chromatography tandem mass spectrometry(UPLC-MS/MS) method for determination of niclosamide residue in soil. Methods The soil sample was extracted ultrasonically by acetonitrile and centrifugated,and then the supernatant was analyzed by UHPLC-MS/MS after filtration,quantitatived by external standard method.Waters BEH C18 chromatographic column was used as stationary phase,and the mixture of methanol and water mixed in different ratios was used as mobile phase in gradient elution. Electrospray negative ion source and multi-reaction monitoring mode were adopted in MS/MS. Results Linear relationship between values of peak area and mass concentration of niclosamide was kept in the range of 0.002 to 0.080 mg/L(r=0.999 6),with the limit of detection was 5×10^(-4) ng and the limit of quantitation(LOQ) was 0.5 μg/kg.At the spiked concentration of 0.02,0.10 and 0.20 mg/kg,mean recoveries from 73.4% to 79.8%,with the relative standard deviation(RSD) ranging from 1.5% to 3.3%. Conclusion The method is simple,efficient,sensitive and accurate,which is suitable for the determination of niclosamide in soil.

关 键 词：超高效液相色谱-串联质谱法 土壤 氯硝柳胺 残留 

分 类 号：R115[医药卫生—公共卫生与预防医学]