Abstract
Objective: In order to analyze the risk of pesticide residues in D. officinale, a method for rapid determination of 56 pesticide residues in D. officinale by a kind of ultrafiltration purification column（MPFC-QuEChERS） combined with ultra-performance liquid chromatography- tandem mass spectrometry（UHPLC-MS/MS）was developed. Methods: The samples were extracted with acetonitrile contained 0.1% formic acid, salted out, shaken, centrifuged, and single-step purified by a MPFC-QuEChERS purification column. Mass spectrometer was operated in the positive and negative ion mode using select reaction monitoring for qualitative and quantitative analysis. Results: The result showed that, the 56 kinds of pesticides showed good linearity when they were in 1.0~250.0 μg/L （R2＞0.99）. The limits of detection （LOD） was 1～5 μg/kg. Three levels of 1, 2 and 10 times of LOQ were added to the sample, the average recovery of each substance in D. officinale was 75.1% to 107.0%, of which the RSDs were 2.7%～18.9%. Conclusion: This method was used to detect pesticide residues in 20 batches of D. officinale. The results showed that 6 kinds of pesticides were detected in 5 samples with the contents ranging from 0.066 7 mg/kg to 1.872 mg/kg. The method is simple, fast and efficient, and could be used for rapid screening and analysis of pesticide residues in D. officinale.
Publication Date
10-20-2023
First Page
48
Last Page
55,84
DOI
10.13652/j.spjx.1003.5788.2022.81008
Recommended Citation
Zhan-bin, LI; Li-jun, ZHAO; Yong-qiao, HUANG; Xue, WANG; and Yang, LU
(2023)
"Rapid determination of 56 pesticide residues in Dendrobium officinale by MPFC-QuEChERS method combined with ultra-performance liquid chromatography-tandem mass spectrometry,"
Food and Machinery: Vol. 39:
Iss.
7, Article 7.
DOI: 10.13652/j.spjx.1003.5788.2022.81008
Available at:
https://www.ifoodmm.cn/journal/vol39/iss7/7
References
[1] 王治丹, 代云飞, 罗尚娟, 等. 铁皮石斛化学成分及药理作用的研究进展[J]. 华西药学杂志, 2022, 37（4）: 472-476.
WANG Z D, DAI Y F, LUO S J, et al. Research progress on chemical constituents and pharmacological effects of Dendrobium officinale[J]. West China Journal of Pharmaceutical Sciences, 2022, 37（4）: 472-476.
[2] 唐靖雯, 彭政忠, 卢礼平, 等. 贵州铁皮石斛叶的质量及安全评价研究[J]. 贵州中医药大学学报, 2022, 44（4）: 21-25.
TANG J W, PENG Z Z, LU L P, et al. Study on quality and safety evaluation of Dendrobium officinale leaves from Guizhou[J]. Journal of Guizhou University of Traditional Chinese Medicine, 2022, 44（4）: 21-25.
[3] 杨婉珍, 康传志, 纪瑞锋, 等. 中药材残留农药情况分析及其标准研制的思考[J]. 中国中药杂志, 2017, 42（12）: 2 284-2 290.
YANG W Z, KANG C Z, JI R F, et al. Situation analysis and standard formulation of pesticide residues in traditional Chinese medicines[J]. China Journal of Chinese Materia Medica, 2017, 42（12）: 2 284-2 290.
[4] 国家药典委员会. 中华人民共和国药典: 四部[S]. 2015版. 北京: 中国医药科技出版社, 2015.
Chinese Pharmacopoeia Commission. Pharmacopoeia of the people's republic of China: Part IV[S]. 2015 Edition. Beijing: China Pharmaceutical Science and Technology Press, 2015.
[5] 范丽丽, 王娟, 吴加伦. 气相色谱法测定铁皮石斛、浙贝母和人参中嘧菌酯残留[J]. 分析科学学报, 2017, 33（2）: 222-226.
FAN L L, WANG J, WU J L. Determination of azoxystrobin residues in Dendrobium officinale, Fritiliariae thumbergii and Panax ginseng by gas chromatography[J]. Journal of Analytical Science, 2017, 33（2）: 222-226.
[6] 郝经文, 徐文冬, 石敏珠, 等. GC-MS同时测定霍山石斛及霍山产铁皮石斛中拟除虫菊酯和氨基甲酸酯类16种农药残留的检测方法[J]. 食品工业科技, 2019, 40（9）: 230-234.
HAO J W, XU W D, ZHI M Z, et al. Simultaneous determination of 16 kinds of pyrethroid and carbamate pesticide residues in Dendrobium huoshanense and Dendrobium officinale from Huoshan by GC-MS[J]. Science and Technology of Food Industry, 2019, 40（9）: 230-234.
[7] 聂静苑. 固相萃取-GC-MS法检测铁皮石斛药材中的5种常见农药残留[J]. 食品与药品, 2018, 20（6）: 422-425.
NIE J Y. Determination of 5 common pesticide residues in Dendrobium officinale by SPE-GC-MS[J]. Food and Drug, 2018, 20（6）: 422-425.
[8] 张权, 毕珊, 吴玉田, 等. Sin-QuEChERS Nano净化柱结合气相色谱—串联质谱法快速筛查石斛中84种农药残留[J]. 色谱, 2022, 40（6）: 565-575.
ZHANG Q, BI S, WU Y T, et al. Rapid screening of 84 pesticide residues in polygonum capitatum by SinQuEChERS Nano purification column with gas chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2022, 40（6）: 565-575.
[9] 周敏, 朱萌萌, 王珍, 等. QuEChERS-VADLLME-内标法-GC-MS/MS快速测定铁皮石斛中农药残留[J]. 食品研究与开发, 2019, 40（16）: 135-145.
ZHOU M, ZHU M M, WANG Z, et al. Study about rapid analysis of pesticide residues in Dendrobium candidum by application of vortex-asisted dispersive liquid-liquid microextraction and QuEChERS and internal standard method coupled with GC-MS/MS[J]. Food Research and Development, 2019, 40（16）: 135-145.
[10] 贾宁, 曾绍东, 陈吴海, 等. 超高效液相色谱—串联质谱法测定铁皮石斛中的吡咯里西啶生物碱[J]. 现代食品科技, 2022, 38（2）: 295-304.
JIA N, ZENG S D, CHEN W H,et al. Determination of pyrrolizidine alkaloids in Dendrobium officinale kimura et migo by UPLC-MS/MS[J]. Modern Food Science & Technology, 2022, 38（2）: 295-304.
[11] 肖苏萍, 钟荣荣, 高慧, 等. 超高效液相色谱—串联质谱法快速测定不同石斛中8种农药残留量[J]. 中国现代中药, 2020, 22（4）: 603-608, 621.
XIAO S P, ZHONG R R, GAO H,et al. Rapid detection of 8 pesticide residues in different Dendrobii Caulis by ultra high performance liquid chromatography-tandem mass spectrometry[J]. Modern Chinese Medicine, 2020, 22（4）: 603-608, 621.
[12] 钟冬莲, 汤富彬, 莫润宏, 等. 分散固相萃取—高效液相色谱—串联质谱法测定铁皮石斛中8种有机磷农药残留[J]. 分析试验室, 2017, 36（5）: 571-575.
ZHONG D L, TANG F B, MO R H, et al. Determination of 8 organophosphorus pesticides in fresh Dendrobium officinale by dispersive solid-phase extraction method and high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Analysis Laboratory, 2017, 36（5）: 571-575.
[13] 张艳. 农药残留分析中不同提取溶剂的评价[J]. 甘肃农业科技, 2006（9）: 28-29.
ZHANG Y. Evaluation different extraction solvent in analysis of pesticide residues[J]. Gansu Agricultural Science and Technology, 2006（9）: 28-29.