Determination of Residues of Diflubenzuron and Chlorbenzuron in Vegetables by High Performance Liquid Chromatography with QuEChERS Purification
摘 要
蔬菜样品被切成小段,分取10.00 g,和10 mL乙腈涡旋混合1 min。加入4.0 g无水硫酸镁和1.0 g氯化钠,涡旋振荡1 min,离心5 min。分取上清液1 mL,分别加入100 mg无水硫酸镁、75 mg C18,涡旋1 min,离心2 min。上清液过0.22 μm滤膜,滤液流经高效液相色谱仪,在ZORBAX SB-C18色谱柱上以体积比45∶55的乙腈-水体系进行等度洗脱。结果显示:除虫脲和灭幼脲的质量浓度均在0.1~5.0 mg·L-1内与其对应的峰面积呈线性关系,检出限(3S/N)分别为0.007,0.02 mg·kg-1;对混合标准溶液进行6次重复测定和6 d连续测定,除虫脲和灭幼脲峰面积的相对标准偏差分别为0.83%,1.6%(日内精密度试验)和2.5%,1.8%(日间精密度试验);以结球甘蓝、菠菜、花椰菜为基质进行3个浓度水平的加标回收试验,回收率为87.4%~104%和75.3%~98.1%。方法用于以上3种共15份蔬菜样品的分析,仅在1个花椰菜样品中检出了除虫脲,检出量(0.014 mg·kg-1)低于相关国家标准规定的残留限量(1 mg·kg-1)。
Abstract
After the vegetable samples were cut into small pieces, an aliquot (10.00 g) was taken and mixed with 10 mL of acetonitrile by swirling for 1 min. Anhydrous magnesium sulfate (4.0 g) and sodium chloride (1.0 g) were added, the mixture was whirled for 1 min, and centrifuged for 5 min. An aliquot (1 mL) of the supernatant was taken, and 100 mg of anhydrous magnesium sulfate together with 75 mg of C18 was added, respectively. After whirling for 1 min and centrifuging for 2 min, the supernatant was passed through a 0.22 μ m filter membrane. The filtrate was introduced into high performance liquid chromatograph, and targets were separated on ZORBAX SB-C18 column with acetonitrile-water system at volume ratio of 45:55 under isocratic elution. As shown by the results, the mass concentrations of diflubenzuron and chlorbenzuron were linearly related with their corresponding peak areas in the range of 0.1-5.0 mg·L-1, with detection limits (3S/N) of 0.007, 0.02 mg·kg-1, respectively. Six repeated determinations and 6 d continuous determinations on the mixed standard solution were made, and RSDs of the peak areas of diflubenzuron and chlorbenzuron were 0.83%, 1.6% (for intra-day precision test) and 2.5%, 1.8% (for inter-day precision test), respectively. Test for the spiked recovery was made at the 3 concentration levels with cabbage, spinach and cauliflower as matrices, giving recoveries in the range of 87.4%-104% and 75.3%-98.1%. The proposed method was applied to the analysis of 15 samples of three kinds of vegetables, and diflubenzuron was detected in one cauliflower sample, and the detection amount (0.014 mg·kg-1) was lower than the residue limit (1 mg·kg-1) stipulated in relevant national standards.
中图分类号 O657.7 DOI 10.11973/lhjy-hx202205021
所属栏目 专题报道(食品质量安全分析)
基金项目 辽宁大学“大学生创新创业训练计划”项目(D202011281212255742);辽宁大学“本科实验教学优秀奖”教改项目;辽宁省博士启动基金(201501131);辽宁省博士启动基金(2020-BS-086)
收稿日期 2021/9/8
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备注安佳,硕士研究生,主要从事环境污染物化学分析
引用该论文: AN Jia,ZHANG Ying,SHENG Yuting,LIU Yifeng,YU Haibo,JING Kui. Determination of Residues of Diflubenzuron and Chlorbenzuron in Vegetables by High Performance Liquid Chromatography with QuEChERS Purification[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2022, 58(5): 603~606
安佳,张营,盛玉婷,刘益丰,于海波,景逵. QuEChERS净化-高效液相色谱法测定蔬菜中除虫脲和灭幼脲的残留量[J]. 理化检验-化学分册, 2022, 58(5): 603~606
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【5】中华人民共和国农业部.水果、蔬菜中杀铃脲等七种苯甲酰脲类农药残留量的测定高效液相色谱法:NY/T 1720-2009[S].北京:中国标准出版社, 2009.
【6】中华人民共和国卫生部,中国国家标准化管理委员会.植物性食品中灭幼脲残留量的测定:GB/T 5009.135-2003[S].北京:中国标准出版社, 2004.
【7】司露露,梁杨琳,李湧,等.QuEChERS-气相色谱串联质谱法快速测定供港蔬菜中118种农药残留[J].化学研究与应用, 2020,32(11):2034-2043.
【8】中华人民共和国国家质量监督检验检疫总局,中国国家标准化管理委员会.水果和蔬菜中450种农药及相关化学品残留量的测定液谱色谱-串联质谱法:GB/T 20769-2008[S].北京:中国标准出版社, 2009.
【9】MUHAMMAD M, JAN M R, SHAH J, et al. Evaluation and statistical analysis of the modified QuEChERS method for the extraction of pinoxaden from environmental and agricultural samples[J]. Journal of Analytical Science and Technology, 2017,8:12.
【10】张爱娟,冯义志,马新刚,等.啶磺草胺和异丙隆在小麦中的残留检测及膳食风险评估[J].农药, 2020,59(11):821-824.
【11】魏进,张盈,王洪瑶,等.QuEChERS-超高效液相色谱-串联质谱法同时检测大米中5种农药残留[J].食品安全质量检测学报, 2021,12(5):1783-1788.
【12】龚敏,孙慧洁,张春冬.QuEchERS-HPLC-MS/MS法测定槟榔中42种农药残留[J].热带农业科学, 2020,40(11):107-114.
【13】李哲,徐冬梅,张兰,等.QuEChERS-超高效液相色谱法测定水样中吡虫啉和虫螨腈[J].农药, 2019,58(4):291-292.
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