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HPLC-MS/MS法测定枇杷中乙螨唑残留量及安全评价
引用本文:王潇楠,常虹,王思威,顾燕萍,孙海滨,刘艳萍.HPLC-MS/MS法测定枇杷中乙螨唑残留量及安全评价[J].中国农学通报,2022,38(22):121-125.
作者姓名:王潇楠  常虹  王思威  顾燕萍  孙海滨  刘艳萍
作者单位:广东省农业科学院植物保护研究所/广东省植物保护新技术重点实验室,广州 510640
基金项目:农业行业标准制定和修订项目“制定乙螨唑在枇杷中的残留限量标准:开展乙螨唑在枇杷上的残留试验”(181821301092372074);广东省农业科学院科技创新战略专项“2018年青年导师制项目”(R2018QD-065)
摘    要:为评价乙螨唑在枇杷上使用的安全性,通过田间试验研究乙螨唑在枇杷上残留消解动态与最终残留量,并进行膳食风险评估。样品经乙腈提取,N-丙基乙二胺(PSA)与十八烷基键合硅胶(C18)组合吸附剂净化,高效液相色谱-三重四级杆串联质谱仪(HPLC-MS/MS)检测,外标法定量。结果表明,在0.01~1.0 mg/kg 3个添加水平下,乙螨唑在枇杷上的平均回收率为89.2%~97.1%,相对标准偏差(RSD)为3.4%~5.3%,定量限(LOQ)为0.01 mg/kg。乙螨唑在枇杷上半衰期为6.9~8.9天,20%乙螨唑悬浮剂(SC)以33.3 mg/kg和50 mg/kg分别施用2、3次,当采收间隔期为14、21与28天时,枇杷中乙螨唑残留量均值依次是0.055~0.37、0.032~0.19、0.014~0.12 mg/kg,可见,随着采收间隔期的延长,枇杷上乙螨唑残留量呈减少趋势。膳食风险评估结果显示,乙螨唑的国家估算每日摄入量(NEDI)是0.0126 mg,风险商(RQ)是0.4%,对一般人群健康不会产生不可接受的风险。

关 键 词:乙螨唑  枇杷  残留与消解动态  膳食风险评估  高效液相色谱-串联质谱法  
收稿时间:2021-07-21

Residue Analysis and Safety Evaluation of Etoxazole in Loquat by HPLC-MS/MS
WANG Xiaonan,CHANG Hong,WANG Siwei,GU Yanping,SUN Haibin,LIU Yanping.Residue Analysis and Safety Evaluation of Etoxazole in Loquat by HPLC-MS/MS[J].Chinese Agricultural Science Bulletin,2022,38(22):121-125.
Authors:WANG Xiaonan  CHANG Hong  WANG Siwei  GU Yanping  SUN Haibin  LIU Yanping
Institution:Institute of Plant Protection, Guangdong Academy of Agricultural Sciences/ Guangdong Provincial Key Laboratory of High Technology for Plant Protection, Guangzhou 510640
Abstract:To evaluate the safety of etoxazole, the dissipation and residue of etoxazole in loquat was studied under field condition, and dietary risk assessment was conducted. The sample was extracted by acetonitrile, purified with PSA and C18, and determined by high performance liquid chromatography tandem triple quadrupole mass spectrometer (HPLC-MS/MS). The mean recovery of etoxazole in loquat was 89.2%-97.1% at the three spiking levels from 0.01 to 1.0 mg/kg, with relative standard deviations (RSD) of 3.4%-5.3%, and the limits of quantitation (LOQ) was 0.01 mg/kg. The half-life of etoxazole in loquat was 6.9-8.9 d. When 20% etoxazole SC was applied at the dosage of 33.3 and 50 mg/kg, for two and three times, respectively, the final residue of etoxazole in loquat was 0.055-0.37, 0.032-0.19 and 0.014-0.12 mg/kg at 14, 21 and 28 d after the last application. The residues of etoxazole in loquat gradually decreased with the extension of harvest interval. Assessing dietary risk found that the national estimated daily intake (NEDI) of etoxazole was 0.0126 mg, risk quotient (RQ) was 0.4%, and there was no unacceptable risk to the health of the general population.
Keywords:etoxazole  loquat  residue and degradation dynamics  dietary risk assessment  HPLC-MS/MS  
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