Please wait a minute...
 
 
食品与发酵工业  2021, Vol. 47 Issue (8): 230-235    DOI: 10.13995/j.cnki.11-1802/ts.025700
  分析与检测 本期目录 | 过刊浏览 | 高级检索 |
QuEChERS结合超高效液相色谱串联质谱法测定花椒中烯效唑残留量及贮藏稳定性
范金平1, 张盈2, 魏进2*, 罗世霞1, 段婷婷2*
1(贵州师范大学 化学与材料科学学院,贵州 贵阳,550025)
2(贵州省农业科学院植物保护研究所,贵州 贵阳,550009)
Determination of uniconazole and storage stability in Zanthoxylum bungeanum Maxim by QuEChERS-UHPLC-MS/MS
FAN Jinping1, ZHANG Ying2, WEI Jin2*, LUO Shixia1, DUAN Tingting2*
1(College of chemistry and materials science, Guizhou Normal University, Guiyang 550025,China)
2(State Key Laboratory for Biology of Plant Diseases and Insect Pests, Institute of Plant Protection, Guizhou Academy of Agricultural Sciences, Guiyang 550009,China)
下载:  HTML   PDF (4901KB) 
输出:  BibTeX | EndNote (RIS)      
摘要 该研究建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography tandem mass spectromentry,UPLS-MS/MS)测定花椒中烯效唑残留量的检测方法,并测定花椒样品中烯效唑残留量以及低温条件下烯效唑在花椒中贮藏稳定性研究。样品经0.1%(体积分数)乙酸乙腈涡旋提取,经PSA+GCB净化剂净化后,采用C18色谱柱分离,在正离子模式下UPLC-MS/MS测定。结果表明,烯效唑溶剂标准曲线和基质标准曲线在1.0~50.0 ng/mL线性良好,相关系数(R2)为0.993 7~0.999 7。在0.02、0.05、0.20 mg/kg 3个添加浓度下,方法的回收率为71.50%~85.98%,相对标准偏差为1.13%~5.36%。烯效唑方法定量限为0.02 mg/kg;花椒在-20 ℃贮藏条件下烯效唑的平均降解率均<30%,说明烯效唑在花椒样品中至少可以稳定贮藏150 d。该方法操作简单、灵敏度高、准确可靠,适用于鲜花椒、干花椒中烯效唑的检测,可为解决烯效唑在食品中残留的安全问题提供技术支撑。
服务
把本文推荐给朋友
加入引用管理器
E-mail Alert
RSS
作者相关文章
范金平
张盈
魏进
罗世霞
段婷婷
关键词:  烯效唑  鲜花椒  干花椒  QuEChERS  超高效液相色谱-串联质谱法    
Abstract: A method for the simultaneous determination of uniconazole in Zanthoxylum bungeanum Maxim by ultra performance liquid chromatography tandem mass spectrometry (UHPLC-MS/MS) was established. The experimental samples were extracted with acetonitrile containing 0.1% acetic acid and purified with PSA and GCB. The mobile phase was eluted with acetonitrile and 0.1% formic acid aqueous solution. The analytes were separated on an Hypersil GOLD C18 column and quantitatively analyzed by the external standard method using matrix-matched calibration curves. The results showed that there was good linearity in the range of 1.0-50 ng/mL under the optimal conditions, with correlation coefficients R2 of 0.993 7-0.999 7. The spiked recoveries of uniconazole in Zanthoxylum bungeanum Maxim at three spiked levels of 0.02, 0.05, 0.20 mg/kg ranged from 71.50% to 85.98%, with relative standard deviations RSDs of 1.13%-5.36%. The limits of quantitation of LOQ were 0.02 mg/kg. Moreover, the average degradation rate of uniconazole in Zanthoxylum bungeanum Maxim was less than 30% at -20 ℃. The established method was simple, sensitive, accurate and reliable, and could meet the requirement of multi pesticide residues analysis in mango skin and flesh. It was of great significance to solve the safety problems for the residue of uniconazole in foods.
Key words:  uniconazole    fresh Zanthoxylum bungeanum Maxim    dried Zanthoxylum bungeanum Maxim    QuEChERS    ultra performance liquid chromatography tandem mass spectromentry
               出版日期:  2021-04-25      发布日期:  2021-05-20      期的出版日期:  2021-04-25
基金资助: 黔农科院基础性公益性专项([2020]15)
作者简介:  硕士(魏进高级实验师和段婷婷正高级实验师为共同通讯作者,E-mail:232512147@qq.com;137829681@qq.com)
引用本文:    
范金平,张盈,魏进,等. QuEChERS结合超高效液相色谱串联质谱法测定花椒中烯效唑残留量及贮藏稳定性[J]. 食品与发酵工业, 2021, 47(8): 230-235.
FAN Jinping,ZHANG Ying,WEI Jin,et al. Determination of uniconazole and storage stability in Zanthoxylum bungeanum Maxim by QuEChERS-UHPLC-MS/MS[J]. Food and Fermentation Industries, 2021, 47(8): 230-235.
链接本文:  
http://sf1970.cnif.cn/CN/10.13995/j.cnki.11-1802/ts.025700  或          http://sf1970.cnif.cn/CN/Y2021/V47/I8/230
[1] 付陈梅, 阚建全, 陈宗道, 等.花椒的成分研究及其应用[J].中国食品添加剂, 2003(4):83-85;122.FU C M, KAN J Q, CHEN Z D, et al.Application of Zanthoxylum and study on its components[J].China Food Addi,2003(4):83-85;122.
[2] 叶倩, 黄健祥, 孙玲, 等.QuEChERS-超高效液相色谱-串联质谱法测定叶类蔬菜中5种植物生长调节剂的残留[J].农药学学报, 2017, 19(5):589-596.YE Q, HUANG J X, SUN L, et al.Determination of five plant growth regulator residues in leafy vegetables by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry[J].Chin J Pestic Sci,2017, 19(5):589-596.
[3] 林海丹, 谢守新, 吴思彦, 等.广东地区果蔬中植物生长调节剂应用现状调查[J].广东农业科学, 2015, 42(12):82-85.LIN H D, XIE S X,WU S Y, et al.Investigation on application situation of plant growth regulators in fruits and vegetables in Guangdong[J].Guangdong Agric Sci, 2015, 42(12):82-85.
[4] 仲伶俐, 胡莉, 郭灵安, 等.固相萃取-超高效液相色谱-串联质谱测定水果中5种植物生长调节剂残留量[J].分析测试学报, 2016, 35(4):466-470.ZHONG L L, HU L, GUO L A, et al.Determination of 5 plant growth regulator residues in fruits by solid phase extraction and ultra high performance liquid chromatography -tandem mass spectrometry[J].Instrum Anal,2016, 35(4):466-470.
[5] 张锋, 潘康标, 田子华.植物生长调节剂研究进展及应用对策[J].现代农业科技, 2012(1):193-195.ZHANG F, PAN K B, TIAN Z H.Research progress and application countermeasures of plant growth regulators[J].Modern Agric Sci Tech,2012(1):193-195.
[6] 刘思洁, 方赤光, 崔勇, 等.植物生长调节剂在植物源性食品中残留量检测技术的研究进展[J].食品安全质量检测学报, 2016, 7(1):8-13.LIU S J,FAN C G,CUI Y.et al.Advances in detection technologies of plant growth regulator residue in plant foods[J].Food Saf Qual,2016,7(1):8-13.
[7] 国家卫生健康委员会, 农业农村部, 国家市场监督管理总局.GB 2763—2019食品安全国家标准 食品中农药最大留限量[S].北京:中国标准出版社, 2019.National Health Commission, Ministry of Agriculture and Rural Affairs, State Administration for Market Regulation.GB 2763—2019 National food safety standard maximum residue limits for pesticides in food National standards of the People's Republic of China[S].Beijing:China Standards Press, 2019.
[8] 徐国锋, 聂继云, 李静, 等.GC/ECD测定葡萄中多效唑和烯效唑的残留[J].农药, 2014, 53(10):736-738;755.XU G F, NIE J Y, LI J, et al.Simultaneous determination of paclobutrazol and uniconazole residues in grape by GC/ECD[J].Agrochemicals, 2014, 53(10):736-738;755.
[9] 张敏, 闫超杰, 付海滨, 等.固相萃取净化-高效液相色谱测定水果中赤霉素、多效唑、烯效唑残留量[J].食品与发酵工业, 2014, 40(2):192-195.ZHANG M, YAN C J, FU H B, et al.Solid phase extraction purification-determination of gibberellins、paclobutrazol and uniconazole residues in fruits by HPLC[J].Food and Fermentation Industries,2014, 40(2):192-195.
[10] 廖强, 杨文钰, 陈兴福, 等.泽泻块茎中烯效唑残留的测定[J].农药, 2008, 47(4):284-285.LIAO Q, YANG W Y, CHEN X F, et al.Mensuration of uniconazol remant in Alisma orientalis(Sam.) Juzep[J].Agrochemicals, 2008, 47(4):284-285.
[11] 徐宜宏, 蒋施, 付海滨, 等.苹果、番茄、玉米中7种植物生长调节剂的气相色谱-串联质谱检测方法[J].农药, 2014, 53(2):113-115.XU Y H, JIANG S, FU H B, et al.Determination of 7 plant growth regulators in apple, tomato, maize by gas chromatography-tandem mass spectrometry[J].J Pesticides,2014,53(2):113-115.
[12] 翟宇瑶, 郭宝林.高效液相色谱-串联质谱测定4种植物生长延缓剂在6种根及根茎类药材中残留量[J].中国中药杂志, 2017, 42(11):2 110-2 116.ZHAI Y Y, GUO B L.HPLC-MS/MS determination of residual amount of 4 plant growth retardants in 6 dried root and rhizome herbs[J].Chin J Chin Mater Med, 2017, 42(11):2 110-2 116.
[13] 师君丽, 孔光辉, 逄涛, 等.超高效液相色谱-电喷雾串联四级杆质谱法快速测定烟草中8种植物生长调节剂残留[J].分析科学学报, 2016, 32(4):510-514.SHI J L, KONG G H, PANG T, et al.Rapid determination of 8 plant growth regulator residues in tobacco by superhigh performance liquid chromatography-electrospray tandem four-stage rod mass spectrometry[J].J Anal Sci,2016, 32(4):510-514.
[14] 中华人民共和国农业部. NY/T 3094—2017 植物源农产品中农药残留储藏稳定性试验准则[S].北京:中国标准出版社, 2019.The Ministry of Agriculture of the People's Republic of China.NY/T 3094—2017 Test criteria for stability of pesticide residue storage in plant-derived agricultural products[S].Beingjing:China Standards Press, 2017.
[15] 孔光辉, 师君丽, 李勇, 等.QuEChERS-UHPLC-MS/MS法测定烟草中硝苯菌酯[J].分析试验室, 2018, 37(9):1 062-1 065.KONG G H, SHI J L, LI Y, et al.Determination of 2、4-DNOPC in tobacco by UHPLC-MS/MS based on QuEChERS[J].Chin J Anal Lab,2018, 37(9):1 062-1 065.
[16] 范金平, 张盈, 魏进, 等.QuEChERS-超高效液相色谱-串联质谱法同时测定芒果中氟吡菌酰胺、肟菌酯及其代谢物残留量[J].农药, 2020, 59(7):516-522.FAN J P, ZHANG Y, WEI J, et al.Determination of fluopyram, trifloxystrobin and its metabolite in mango by QuEChERS-UHPLC-MS/MS[J].J Pesticides,2020, 59(7):516-522.
[17] 刘亚伟, 董一威, 孙宝利, 等.QuEChERS在食品中农药多残留检测的应用研究进展[J].食品科学, 2009, 30(9):285-289.LIU Y W, DONG Y W, SUN B L, et al.Summary of application of QuEChERS method in multi-residue determination of pesticides in food[J].Food Sci, 2009, 30(9):285-289.
[18] 张景. HPLC法同时测定大麻花及叶中5种大麻素类成分的含量[J].中药材, 2019, 42(8):1 824-1 827.ZHANG J.Determination of five cannabinoids in flowers and leaves of cannabis stativa by HPLC[J].Journal of Chinese Medicinal Materials, 2019, 42(8):1 824-1 827.
[19] 林涛, 邵金良, 刘兴勇, 等.超高效液相色谱-串联质谱法测定热带水果中杀虫双残留[J].色谱, 2018, 36(12):1 223-1 227.LIN T, SHAO J L, LIU X Y, et al.Determination of bisultab residue in tropical fruits by ultra performance liquid chromatography-tandem mass spectrometry[J].Chin J Chromatogr,2018, 36(12):1 223-1 227.
[20] 谢景丽, 李凌云, 刘新艳, 等.改进的QuEChERS-液相色谱串联质谱法快速测定中草药中147种农药残留[J].农产品质量与安全, 2016(2):65-69.XIE J L, LI L Y, LIU X Y, et al.An improved QuEChERS-liquid chromatography tandem mass spectrometry method was developed for the rapid determination of 147 pesticide residues[J]. Qual Saf Agro-Products,2016(2):65-69.
[21] 中华人民共和国农业农村部. NY/T 788—2018 农药残留试验准则[S].北京:中国标准出版社, 2018.Ministry of Agriculture and Rural Affairs of the People's Republic of China.NY/T 788—2018 Guideline on pesticide residue trials[S].Beingjing:China Standards Press, 2018.
[1] 吕青骎, 王玮, 梁丽姣, 滕爽, 徐幸莲. QuEChERS结合超高效液相色谱质谱法测定禽蛋及其制品中42种农药及其代谢物[J]. 食品与发酵工业, 2020, 46(5): 255-262.
[2] 徐鹏, 赵建珍, 闫伟伟, 罗慧玉, 陈佳琛, 刘慧. QuEChERS-气相色谱-串联质谱法测定番茄中九种甲氧基丙烯酸酯类杀菌剂[J]. 食品与发酵工业, 2020, 46(21): 242-246.
[3] 马凯, 蔡芳叶, 黄永桥, 吴新文, 杨昌彪, 李占彬. 超高效液相色谱-串联质谱法检测蜂蜜中九种氨基糖苷类药物残留[J]. 食品与发酵工业, 2020, 46(18): 203-208.
[4] 张伟彪, 顾亚萍, 曾定玲, 王瑞, 林慧纯, 尹义捐, 方长发. 三种常用溶剂对98种农残检测结果稳定性的影响[J]. 食品与发酵工业, 2020, 46(16): 236-242.
[5] 金婷, 孙欣, 李卓瓦, 冯晓慧, 谭胜兵, 王明林. QuEChERS-气相色谱-三重四级杆质谱法检测石榴中的19种含磷农药残留[J]. 食品与发酵工业, 2019, 45(3): 275-280.
[6] 黄胜广, 赵卉, 王玉方, 金美伶, 宋超, 王峰. QuEChERS结合超高效液相色谱-串联质谱法同时测定梅花鹿鹿茸中18种磺胺[J]. 食品与发酵工业, 2019, 45(24): 223-228.
[7] 毕思远, 曹建涛, 李保玲, 朱志强, 曹涛, 李森. QuEChERS-气相色谱分析厦门海域鱼体中有机氯类农药残留特征及风险评价[J]. 食品与发酵工业, 2019, 45(21): 229-235.
[8] 李建勋, 范蓓, 周杰, 甄云鹏, 单吉浩. QuEChERS-超高效液相色谱-飞行时间质谱法快速筛查蔬菜中154种农药残留[J]. 食品与发酵工业, 2019, 45(19): 239-250.
[9] 黄坤, 范小龙, 曹琦, 韩智, 张莉, 王会霞, 郭嘉. QuEChERS -超高效液相色谱串联质谱法快速测定禽蛋中7种喹诺酮类兽药残留[J]. 食品与发酵工业, 2019, 45(16): 261-265.
[10] 宋佳, 李锦清, 李聪, 周勇, 黄翠莉, 綦艳. QuEChERS萃取-液相色谱法测定酱油和酱制品中三氯蔗糖[J]. 食品与发酵工业, 2019, 45(14): 229-232.
[11] 鲍鏖天, 裴少芬, 唐杏燕, 等. QuEChERS 结合高效液相色谱串联质谱快速检测速溶茶粉中八种农药残留 [J]. 食品与发酵工业, 2018, 44(5): 232-236.
[12] . QuEChERS- 超高效液相色谱串联质谱法同时测定蜂蜜中 21 种磺胺类药物残留[J]. 食品与发酵工业, 2018, 44(4): 226-233.
[13] 李艳美,粟有志,李芳,雷红琴,袁小雯,张凯丽,杨洁. QuEChERS前处理高效液相色谱法同时测定酵母产品中7种合成酚类抗氧化剂[J]. 食品与发酵工业, 2017, 43(5): 198-.
[14] 池连学,李锋,王永丽,张禧庆,张敏. 采用超高效液相色谱-串联质谱结合改良QuEChERS方法快速分析农产品中天然除虫菊酯6种成分残留[J]. 食品与发酵工业, 2016, 42(7): 209-.
[15] 李培培,陈敏,王军. QuEChERS-高效液相色谱法检测红葡萄酒中多菌灵和甲霜灵杀菌剂残留[J]. 食品与发酵工业, 2015, 41(1): 202-.
No Suggested Reading articles found!
Viewed
Full text


Abstract

Cited

  Shared   
  Discussed   
版权所有 © 《食品与发酵工业》编辑部
地址:北京朝阳区酒仙桥中路24号院6号楼111室
本系统由北京玛格泰克科技发展有限公司设计开发  技术支持:support@magtech.com.cn