Determination of myclobutanil and difenoconazole residues in pollen and honey of litchi by high performance liquid chromatography-tandem mass spectrometry

doi:10.3724/SP.J.1123.2017.09034

Abstract

Abstract:

An effective method was developed for the determination of two major fungicides including myclobutanil and difenoconazole residues in pollen and honey of litchi by modified QuEChERS-high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). The pollen and honey samples were all extracted by acetonitrile, the pollen samples were cleaned-up by 0.9 g anhydrous magnesium sulfate (MgSO₄), 0.15 g primary secondary amine (PSA) and 0.15 g C₁₈; the honey samples were cleaned-up by 0.9 g MgSO₄ and 0.15 g PSA. The 0.1% (v/v) formic acid aqueous solution-acetonitrile (25:75, v/v) were used as the mobile phases. The extracts were separated on a Poroshell-120 EC-C₁₈ chromatographic column, the positive electrospray ion (ESI⁺) source and selected ion monitoring (SIM) mode were used. The analytes were quantified by the matrix matching standard solutions. The matrix matched standard solutions of myclobutanil and difenoconazole showed good linearities in the range of 1-100 μg/L, and the correlation coefficients (r²) were all above 0.9990. The limits of detection (LODs) of myclobutanil and difenoconazole were 0.25 μg/kg and 0.50 μg/kg, respectively. The limits of quantification (LOQs) of myclobutanil and difenoconazole were 0.83 μg/kg and 1.7 μg/kg, respectively. The average recoveries of myclobutanil and difenoconazole in pollen and honey samples were 87.0%-95.2% and 90.1%-96.4% with the relative standard deviations of 1.2%-3.6% and 0.7%-4.1%, respectively. The method is quick, easy and sensitive, and it is suitable for the rapid determination and trace analysis of myclobutanil and difenoconazole in pollens and honeys of litchi. The method can provide data support for the exposure risk assessment of bees and other pollination insects.

Key words: difenoconazole, high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS), myclobutanil, pollen and honey of litchi, QuEChERS

CLC Number:

O658

WANG Siwei, LIU Yanping, SUN Haibin, DU Lanjuan, XU Nengli. Determination of myclobutanil and difenoconazole residues in pollen and honey of litchi by high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(1): 17-22.

References

[1] Bai H Q, Wu J G, Pan X B. Journal of Fruit Science, 2016, 33(4):436白慧卿, 吴建国, 潘学标. 果树学报, 2016, 33(4):436
[2] Huang C X, Wu D Y, Jiang D G, et al. Journal of South China Normal University Natural (Science Edition), 1984(1):49黄昌贤, 吴定尧, 江杜规, 等. 华南师范大学学报(自然科学版), 1984(1):49
[3] Zhang N, Zhang C Q, Zhu G N, et al. Chinese Journal of Pesticide Science, 2016, 18(3):387张宁, 张传清, 朱国念, 等. 农药学学报, 2016, 18(3):387
[4] Wang Y J, Gao J L, Han W S, et al. Journal of Environmental Entomology, 2017, 39(1):126王雅珺, 高景林, 韩文素, 等. 环境昆虫学报, 2017, 39(1):126
[5] Cang T, Zhao X P, Zhang Z H, et al. Zhejiang Agricultural Science, 2009(4):785苍涛, 赵学平, 张志恒, 等. 浙江农业科学, 2009(4):785
[6] Deng Z B, Hu J Y, Qin D M, et al. Chromatographia, 2010, 71(7/8):679
[7] Zhang X Y, Dai X F, Mao J, et al. Chinese Journal of Pesticide Science, 2013, 15(1):91张雪燕, 代雪芳, 毛佳, 等. 农药学学报, 2013, 15(1):91
[8] Mohapatra S. Environ Sci Pollut R, 2016, 23(6):5795
[9] Xue J Y, Chen X C, Jiang W Q, et al. J Chromatogr B, 2015, 975:9
[10] Zhao F F, Zheng X H, Lv D Z, et al. Journal of Henan Agricultural University, 2017, 51(1):115赵方方, 郑雪红, 吕岱竹, 等. 河南农业大学学报, 2017, 51(1):115
[11] Szpyrka E, Walorczyk S. J Environ Sci Heal B, 2017, 52(2):131
[12] Zhao C J, Pang J, Gao W H. Journal of Chinese Institute of Food Science and Technology, 2015, 15(3):175赵春娟, 庞军, 高文惠. 中国食品学报, 2015, 15(3):175
[13] Ferreira J A, Santos L F S, Souza N R S, et al. Bull Environ Contam Toxicol, 2013, 91(2):160
[14] Raeppel C, Nief M, Fabritius M, et al. J Chromatogr A, 2011, 1218(44):8123
[15] Xie J J, Chen J, Li J, et al. Journal of Food Safety and Quality, 2013, 4(1):82谢建军, 陈捷, 李菊, 等. 食品安全质量检测学报, 2013, 4(1):82
[16] Liu Y N, Li W Z, Wei P, et al. Journal of Ecology and Rural Environment, 2016, 32(5):832刘雅楠, 李文卓, 魏鹏, 等. 生态与农村环境学报, 2016, 32(5):832
[17] Guo Y Y, Shi H M, Han X M, et al. Chinese Journal of Analysis Laboratory, 2017, 36(7):811郭亚芸, 史红梅, 韩晓梅, 等. 分析试验室, 2017, 36(7):811
[18] Xue X H, Dai S H, Zhang L S, et al. Chinese Journal of Pesticide Science, 2010, 12(3):309薛晓航, 戴守辉, 张璐珊, 等. 农药学学报, 2010, 12(3):309
[19] Yao F, Song Z Y, Nie J, et al. Physical Testing and Chemical Analysis Part B:Chemical Analysis, 2017, 53(6):650姚芳, 宋志宇, 聂晶, 等. 理化检验-化学分册, 2017, 53(6):650
[20] Su S F, Xue X, Wang J, et al. Chemical Research and Application, 2014, 26(3):460宿书芳, 薛霞, 王骏, 等. 化学研究与应用, 2014, 26(3):460
[21] Chen J H, Wang H L, Guo B Y, et al. Int J Environ An Ch, 2014, 94(8):791
[22] Zhang X Z, Zhao Y C, Luo F J, et al. Journal of Instrumental Analysis, 2016, 35(11):1376张新忠, 赵悦臣, 罗逢健, 等. 分析测试学报, 2016, 35(11):1376
[23] Wang Y, Wang C W, Gao J, et al. China Journal of Chinese Materia Medica, 2014, 39(13):2464王燕, 王春伟, 高洁, 等. 中国中药杂志, 2014, 39(13):2464
[24] Montagner C C, Vidal C, Acayaba R D, et al. Anal Methods, 2014, 6(17):6668
[25] Yang A, EI-Aty A M A, Park J H, et al. Biomed Chromatogr, 2014, 28(6):735
[26] Zhang X Z, Luo F J, Chen Z M, et al. Chinese Journal of Analytical Chemistry, 2013, 41(2):215张新忠, 罗逢健, 陈宗懋, 等. 分析化学, 2013, 41(2):215
[27] Hingmire S, Oulkar D P, Utture S C, et al. Food Chem, 2015(176):145
[28] Yuan Y S. Chinese Pharmaceutical Journal, 1984, 19(6):28袁倚盛. 中国药学杂志, 1984, 19(6):28