摘要
目的建立黄花菜中甲基硫菌灵及其代谢物多菌灵的检测方法,并对黄花菜中的残留量进行膳食摄入风险评估,评价其食用安全性。方法采用乙腈提取黄花菜中甲基硫菌灵及其代谢物多菌灵,N-丙基乙二胺(primary secondary amine,PSA)净化,离心后上清液过滤膜,高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)检测。结果甲基硫菌灵和多菌灵的检出限为1×10^(‒3) ng,定量限为0.01 mg/kg,甲基硫菌灵在黄花菜(鲜)和黄花菜(干)中的添加回收率分别为84%~105%和101%~105%;多菌灵在黄花菜(鲜)和黄花菜(干)中的添加回收率分别为86%~96%和93%~99%。2020年在湖南省和江苏省两地,甲基硫菌灵在黄花菜(鲜)和黄花菜(干)的降解半衰期分别为0.85、0.97 d和0.40、1.65 d;多菌灵在黄花菜(鲜)和黄花菜(干)的降解半衰期分别为1.62、1.88 d和1.66、1.88 d;不同施药次数、施药剂量及采收间隔期,甲基硫菌灵在黄花菜(鲜)和黄花菜(干)的最终残留量分别为<0.01~0.33 mg/kg和<0.01~1.51 mg/kg;多菌灵在黄花菜(鲜)和黄花菜(干)的最终残留量分别为<0.01~2.72 mg/kg和0.052~2.99 mg/kg。结论36%甲基硫菌灵悬浮剂按推荐剂量(675 ga.i./ha)施药3~4次、施药间隔7 d、推荐安全间隔期3 d,甲基硫菌灵(甲基硫菌灵和多菌灵之和,以多菌灵表示)的普通人群国家估算每日摄入量为1.19 mg,占每日允许摄入量的63.1%,不会对一般人群健康产生造成不可接受风险。
Objective To establish an analytical method for the residues of thiophanate-methyl and its metabolite carbendazim in Hemerocallis citrina Baroni,and assess the risk of dietary intake for residues in Hemerocallis citrina Baroni,and evaluate its safety.Methods The thiophanate-methyl and its metabolites carbendazim were extracted with acetonitrile,primary secondary amine(PSA)was used for purification,centrifugated,the supernatant was filtered through the membranes,and analyzed by high performance liquid chromatography-tandem mass spectrometry(HPLC-MS/MS).Results The limits of detection and limits of quantitation of thiophanate-methyl and its metabolite carbendazim were 1×10^(‒3) ng and 0.01 mg/kg,respectively,the recoveries of thiophanate-methyl from the Hemerocallis citrina Baroni(fresh)and Hemerocallis citrina Baroni(dry)were 84%‒105%and 101%‒105%,respectively;the recoveries of carbendazim from the Hemerocallis citrina Baroni(fresh)and Hemerocallis citrina Baroni(dry)were 86%‒96%and 93%‒99%,respectively.In 2020,the the degradation half-lives of thiophanate-methyl in Hemerocallis citrina Baroni(fresh)and Hemerocallis citrina Baroni(dry)in 2 experiment sites of Hunan and Jiangsu were 0.85,0.97 d and 0.40,1.65 d,respectively;and the degradation half-lives of carbendazim in Hemerocallis citrina Baroni(fresh)and Hemerocallis citrina Baroni(dry)in the 2 experiment sites were 1.62,1.88 d and 1.66,1.88 d,respectively,under different application frequency,application dose and harvesting interval,the final residues of thiophanate-methyl in Hemerocallis citrina Baroni(fresh)and Hemerocallis citrina Baroni(dry)were<0.01‒0.33 and<0.01‒1.51 mg/kg,respectively;the final residues of carbendazim in Hemerocallis citrina Baroni(fresh)and Hemerocallis citrina Baroni(dry)were<0.01‒2.72 and 0.052‒2.99 mg/kg,respectively.Conclusion Under the conditions of 36%thiophanate-methyl suspension,3-4 times at the recommended dose(active ingredient 675 ga.i./ha),7 d interval and 14 d recommended safety interval,the international estimated daily intake of thiophanate-methyl(the sum of thiobacillazim methyl and carbendazim,represented by carbendazim)for the general population is 1.19 mg,63.1%of the acceptable daily intake,and does not pose an unacceptable risk to the health of the general population.
作者
孙星
刘川静
杨邦保
耿韧华
王冬兰
SUN Xing;LIU Chuan-Jing;YANG Bang-Bao;GENG Ren-Hua;WANG Dong-Lan(Jiangsu Key Laboratory for Food Quality and Safety-State Key Laboratory Cultivation Base,Ministry of Science and Technology,Nanjing 210014,China)
出处
《食品安全质量检测学报》
CAS
北大核心
2022年第12期3907-3915,共9页
Journal of Food Safety and Quality
基金
国家自然科学基金项目(31772197)。
关键词
甲基硫菌灵
多菌灵
黄花菜
残留
膳食摄入风险评估
thiophanate-methyl
carbendazim
Hemerocallis citrina Baroni
residues
risk assessment of dietary intake
