Safety Monitoring

Rapid determination of 47 kinds of pesticide residues in Ginseng Radix et Rhizoma by Sin-QuEChERS-GC-MS/MS*

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  • 1. Dalian Center for Food and Drug Control and Certification, Dalian 116037, China;
    2. College of Life Science, Nankai University, Tianjin 300071, China

Received date: 2022-03-25

  Online published: 2024-06-26

Abstract

Objective: To establish a rapid analysis method of Sin-QuEChERS technology combined with gas chromatography-tandem mass spectrometry (GC-MS/MS) to detect 47 pesticide residues in Ginseng Radix et Rhizoma. Methods: Ginseng Radix et Rhizoma powder was treated with water and extracted with 1% formic acid-acetonitrile, salted out by the QuEChERS package and purified with Sin-QuEChERS tube in one step, after concentrating internal standard triphenyl phosphate was added, then detected by GC-MS/MS. DB-5MS column was used, the inlet temperature was set to 250 ℃, the initial velocity was 1.2 mL·min-1, the electron impact ion source was applied with multiple reaction monitoring (MRM) modes, and internal standard method was used for quantification. Results: The 47 target compounds showed good linearities within a certain content ranges, with the correlation coefficients (r2) above 0.993 1. At the low, medium, and high addition levels, the average recoveries were in the range of 72.5%-116.0% with the relative standard deviations (RSDs) within 0.70%-13.9%. And the limits of quantitation (LOQs) for the 47 compounds were 0.01 mg·kg-1. Thirty batches of Ginseng Radix et Rhizoma samples were tested and nine pesticides were detected, among them, quintozene showed the highest detection rate of 56.7%. Conclusion: The detecting method is efficient, sensitive, and accuracy, which can be used for rapid screening and quantitative detection of various pesticide residues in ginseng, and has strong practical value.

Cite this article

GAO Na, QIAO Ying, LIU Xue-hong, LI Jun, GE Xiang-wu, SUN Nan, ZHU Dian-long, RUAN Wei-bin, ZHENG Li-xin . Rapid determination of 47 kinds of pesticide residues in Ginseng Radix et Rhizoma by Sin-QuEChERS-GC-MS/MS*[J]. Chinese Journal of Pharmaceutical Analysis, 2022 , 42(12) : 2145 -2154 . DOI: 10.16155/j.0254-1793.2022.12.11

References

[1] 王立岩, 田义新, 李海涛, 等. 基于益气固脱功效的人参药材质量评价的探讨[J].中国中药杂志, 2012,37 (13): 2030
WANG LY, TIAN YX, LI HT, et al. Study on quality evaluation of Panax ginseng based on effects for replenishing Qi and preventing exhaustion[J].Chin J Chin Mater Med, 2012, 37 (13): 2030
[2] 宋齐. 人参化学成分和药理作用研究进展[J].人参研究, 2017,29(2): 47
SONG Q. Research progress on chemical constituents of Panax ginseng and their pharmacological effects[J].Ginseng Res, 2017, 29(2): 47
[3] 马雯, 薛晓利, 秦雪梅, 等. 中药材农药残留及脱除方法研究进展[J].中草药, 2018, 49(2):745
MA W, XUE XL, QIN XM, et al. Research progress on pesticide residues in Chinese medicinal materials and pesticide removal methods[J].Chin Tradit Herb Drugs, 2018, 49(2): 745
[4] 王莹, 王赵, 岳志华, 等. 国产人参中农药残留风险评估[J].中国中药杂志, 2019, 44(7): 1327
WANG Y, WANG Z, YUE ZH, et al. Risk assessment of pesticide residues in domestic ginsengs[J].Chin J Chin Mater Med, 2019, 44(7): 1327
[5] 兰丰, 李晓亮, 段小娜, 等. 固相萃取-超高效液相色谱-串联质谱法测定美国进口水果中15种高风险农药及助剂残留[J].农药学学报, 2019, 21(4):475
LAN F, LI XL, DUAN XN, et al. Determination of 15 high-risk pesticide and adjuvant residues in fruits from USA by solid phase extraction-ultra performance liquid chromatography-tandem mass spectrometry[J].Chin J Pestic Sci, 2019, 21(4):475
[6] 王姗姗, 李刚, 高丽娜, 等.液液萃取分离-气相色谱-串联质谱法同时测定水中12种有机氯农药[J].理化检验,2016,52(4):384
WANG SS, LI G, GAO LN, et al. GC-MS/MS determination of 12 organochlorine pesticides in water with separation by liquid-liquid extraction[J].Phys Testing Chem Anal, 2016, 52(4):384
[7] 孙鹏, 高玉玲, 王金梅, 等. 漂浮固化分散液-液微萃取-气相色谱法测定液态奶中5种拟除虫菊酯类农药残留[J].农药学学报, 2016,18(4):497
SUN P, GAO YL, WANG JM, et al. Dispersive liquid-liquid microextraction based on the solidification of a floating organic droplet followed by gas chromatography for the determination of five pyrethroid pesticides residues in liquid milk samples[J].Chin J Pestic Sci, 2016, 18(4): 497
[8] 王娇, 齐沛沛, 虞淼, 等. 基于功能磁性材料和固相微萃取净化富集一体化的茶饮料中三唑类农药残留分析[J].农药学学报, 2021, 23(6):1168
WANG J, QI PP, YU M, et al. Triazole pesticide residues analysis based on functionalized magnetic materials and solid phase microextraction collaborative technology in tea drinks[J].Chin J Pestic Sci, 2021, 23(6):1168
[9] 宾婕, 王以鑫, 胡建林, 等. QuEChERS-UPLC-MS/MS法快速测定香茅草中33种农药残留量[J].药物分析杂志, 2021, 41(3): 466
BIN J, WANG YX, HU JL, et al. Determination of 33 pesticide residues in Cymbopogon citratus by modified QuEChERS method and UPLC-MS/MS[J].Chin J Pharm Anal, 2021, 41(3):466
[10] 王晓园, 李志梅, 谢循策, 等. QuEChERS-气相色谱-质谱联用法测定山药中50种农药残留[J].药物分析杂志, 2021, 41(11): 1979
WANF XY, LI ZM, XIE XC, et al. Determination of 50 pesticide residues in Chinese Yam by QuEChERS-gas chromatography-tandem mass spectrometry[J].Chin J Pharm Anal, 2021, 41(11):1979
[11] 黄合田, 谢双, 徐祥婷, 等. Sin-QuEChERS结合超高效液相色谱-高分辨质谱法快速筛查绿茶中农药及代谢物残留[J].分析化学, 2020, 48(3): 423
HUANG HT, XIE S, XU XT, et al. Rapid screening of pesticide and metabolites residues in green tea by Sin-QuEChERS with ultra performance liquid chromatography-high resolution mass spectrometry[J].Chin J Anal Chem, 2020, 48(3): 423
[12] 兰韬, 初侨, 郝东宇, 等. Sin-QuEChERS结合UPLC-MS/MS同时检测茶叶中10种有机磷农药残留[J].质谱学报, 2019, 40(3):268
LAN T, CHU Q, HAO DY, et al. Simultaneously detection of 10 organophosphorus pesticides residues in tea by Sin-QuEChERS with UPLC-MS/MS[J].J Chin Mass Spectro Soc, 2019, 40(3): 268
[13] 孙程鹏, 许炳雯, 高娜, 等. Sin-QuEChERS结合超高效液相色谱串联质谱法同时检测果蔬中5种双酰胺类杀虫剂[J].食品安全质量检测学报, 2020, 11(6):1784
SUN CP, XU BW, GAO N, et al. Simultaneous determination of 5 kinds of diamide insecticides in fruits and vegetables by Sin-QuEChERS with ultra performance liquid chromatography tandem mass spectrometry[J].J food Saf Qual Inspect, 2020, 11(6):1784
[14] 郝东宇, 席兴军, 初侨, 等. 快速滤过型净化法结合高效液相色谱-串联质谱同时检测人参中的5种农药残[J].农药学学报, 2019, 21(1): 82
HAO DY, XI XJ, CHU Q, et al. Simultaneous detection of five pesticide residues in ginseng by multi-plug filtration cleanup method combined with high performance liquid chromatography-tandem mass spectrometry[J].Chin J Pestic Sci, 2019, 21(1): 82
[15] 王莹, 王赵, 乔菲, 等. 基于点评估方法的人参中农药残留摄入暴露风险研究[J].中国药事, 2018,32(10):1342
WANG Y, WANG Z, QIAO F, et al. On exposure risk of pesticide residues in ginseng based on deterministic approach[J].Chin Pharm Aff, 2018, 32(10):1342
[16] 孙海, 钱佳奇, 张小波, 等. 人参农药残留研究进展中[J].中国中药杂志, 2022,47(6):1427
SUN H, QIAN JQ, ZHANG XB, et al. Research progress on pesticide residues of Panax ginseng[J].Chin J Chin Mater Med, 2022,47(6):1427
[17] 中华人民共和国药典2020年版.四部[S].2020:275
ChP 2020 Vol Ⅳ[S].2020: 275
[18] 国家药典委员会. 中华人民共和国药典2020年版.一部[S].2020:9
ChP 2020 Vol Ⅰ[S].2020: 9
[19] 宋莉, 周培培, 李阳, 等. 云南玉溪地区烟田根结线虫的SCAR鉴定、分布及其生物防治研究[J].农业资源与环境学报, 2019, 36(4): 546
SONG L, ZHOU PP, LI Y, et al. Distribution of Meloidogyne spp. in tobacco field of Yuxi, Yunnan Province and biological control against Meloidogyne spp.[J].J Agric Res Environ, 2019, 36(4):546
[20] SHAN SJ, WANG WW, SONG CX, et al. The symbiotic bacteria Alcaligenes faecalis of the entomopathogenic nematodes Oscheius spp. exhibit potential biocontrol of plant-and entomopathogenic fungi[J].Microb Biotechnol, 2019, 12(3):45
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