目的: 建立分散固相萃取（QuEChERS）快速样品前处理技术结合超高效液相色谱-串联质谱（UPLC-MS/MS）同时测定香茅草中33 种农药残留的方法。方法: 以乙腈为溶剂, 高速匀浆提取, 经 C18/PSA 小柱及改良的 QuEChERs 填料净化。方法采用Penomenex Kinetex XB-C18 色谱柱（100 mm×2. 1 mm, 1. 7 μm）, 以 0. 1% 甲酸（含 5 mmol·L-1 乙酸铵）溶液和乙腈为流动相进行梯度洗脱, 电喷雾电离源（ESI）, 正离子模式下多反应监测（MRM）。结果: 14 批样品中共检出农药 5种, 1 个样品检出咪鲜胺（3. 12 mg·kg-1）、多菌灵（0. 051 8 mg·kg-1）、吡虫啉（0. 035 1 mg·kg-1）、烯酰吗啉（17. 6 mg·kg-1）和甲基硫菌灵（0. 047 1 mg·kg-1）;另外2 个样品检出多菌灵（0. 015 7 mg·kg-1 和0. 012 9 mg·kg-1）, 其余样品均未检出残留农药, 合格率 64. 3%。33 种待测指标成分线性关系良好, 相关系数均大于 0. 995, 两水平加样回收率全部指标在64. 4%~114. 7%, RSD 为1. 2%~9. 6%, 检测下限为 1. 0~5. 0 μg·kg-1, 符合多农残的痕量分析检测要求。结论: 该方法有针对性地对香茅草中33 种农药残留进行快速筛查与准确检测, 适用于对中药香茅草的日常监控, 同时为基质类似中药的农药残留方法提供借鉴。
[1] 张爱芝, 王全林, 曹丽丽, 等. QuEChERS-超高效液相色谱-串联质谱法测定蔬菜中 250 种农药残留[J]. 色谱, 2016, 34(2): 158
ZHANG AZ, WANG QL, CAO LL, et al. Determination of 250 pesticide residues in vegetables by QuEChERS-High-performance liquid chromatography-tandem mass spectrometry[J]. Chin J Chromatogr, 2016, 34(2): 158
[2] GB 2763—2016 食品安全国家标准食品中农药最大残留限量[S]. 2016
GB 2763—2016Maximum Residue Limit of Pesticide in National Standard Food for Food Safety: GB 2763—2016[S]. 2016
[3] GB 2763. 1—2018 食品安全国家标准食品中百草枯等 43 种农药最大残留限量[S]. 2018
GB 2763. 1—2018 Maximum Residue Limits of Paraquat and Other 43 Pesticides in National Standard Food for Food Safety[S]. 2018
[4] 孔令军, 张娅婷, 谷令彪, 等. 中药材农药残留的研究进展[J]. 中国实验方剂学杂志, 2015, 21(21): 231
KONG LJ, ZHANG YT, GU LB, et al. Research progress of traditional Chinese medicine pesticide residues[J]. Chin J ExpTradit Med Form, 2015, 21(21): 231
[5] 王莹, 金红宇, 孙磊, 等. 中药材中198 种农药残留测定样品前处理平台的建立[J]. 药物分析杂志, 2011, 31(12): 2199
WANG Y, JIN HY, SUN L, et al. Research of pretreatment platform for simultaneous determination of 198 pesticides in traditional Chinese medicine[J]. Chin J Pharm Anal, 2011, 31(12): 2199
[6] 陈丽娜, 宋凤瑞, 刘志强. 液相色谱-质谱联用技术在中药农药残留分析中的应用进展[J]. 质谱学报, 2010, 31(6): 342
CHEN LN, SONG FR, LIU ZQ. Advances on traditional Chinese medicine application of liquid chromatography-tandem mass spectrometry and correspondingly sample preparations in pesticide residue analysis[J]. J Chin Mass Spectrom Soc, 2010, 31(6): 342
[7] 陈溪, 程磊, 曲世超, 等. QuEChERS-液相色谱-质谱法快速筛查和确证大米中 205 种农药残留[J]. 色谱, 2015, 33(10): 1080
CHEN X, CHENG L, QU SC, et al. Rapid screening and confirmation of 205 pesticide residues in rice by QuEChERS and liquid chromatography-mass spectrometry[J]. Chin J Chromatogr, 2015, 33(10): 1080
[8] 崔春艳, 张红医, 吴兴强, 等. 固相萃取-液相色谱-飞行时间质谱法快速筛查与确证谷物和果蔬中 25 种杀菌剂残留[J]. 分析化学, 2017, 45(8): 1195
CUI CY, ZHANG HY, WU XQ, et al. Rapid determination of 25 kinds of fungicides in cereals, fruits and vegetables by solid phase extraction and liquid chromatography coupled with quadrupole-time of flight mass spectrometry[J]. Chin J Anal Chem, 2017, 45(8): 1195
[9] 郑永权. 农药残留研究进展与展望[J]. 植物保护, 2013, 39(5): 90
ZHENG YQ. Development and prospects of the research on pesticide residues[J]. Plant Protect, 2013, 39(5): 90
[10] 杨柳, 王贵禧, 樊金拴. 农产品中农药残留的标准、检测和降解技术的研究进展[J]. 中国农学通报, 2005, 21(12): 108
YANG L, WANG GX, FAN JS. Advances in research on the standards, techniques of determination and degradation of pesticide residues in farm products[J]. Chin Agric Sci Bull, 2005, 21(12): 108
[11] 金红宇, 戴博, 田金改, 等. 中药中外源性有害残留物的控制[J]. 中国药事, 2007, 21(12): 1014
JIN HY, DAI B, TIAN JG, et al. Control of extrinsic harmful residues in traditional Chinese medicine[J]. Chin Pharm Aff, 2007, 21(12): 1014
[12] XU R, WU JW, LIU YG, et al. Analysis of pesticide residues using the quick easy cheap effective rugged and safe(QuEChERS) pesticide multiresidue method in traditional Chinese medicine by gas chromatography with electron capture detection[J]. Chemosphere, 2011(7): 908
[13] 朱峰, 于洁, 霍宗利, 等. QuEChERS-超高效液相色谱-四极杆飞行时间质谱法检测青菜中 214 种农药残留[J]. 中国食品卫生杂志, 2020, 32(1): 25
ZHU F, YU J, HUO ZL, et al. QuEChERS-high-performance liquid chromatography-four-pole Time-of-flight mass spectrometry for the determination of 214 pesticide residues in green vegetables[J]. Chin J Food Hyg, 2020, 32(1): 25
[14] 李蓉, 储大可, 张朋杰, 等. QuEChERS/HPLC-MS/MS 法测定黄瓜、菜心、葡萄、香蕉中 127 种农药残留[J]. 分析测试学报, 2015, 34(5): 502
LI R, CHU DK, ZHANG PJ, et al. Determination of 127 pesticide residues in cucumber, Chinese flowering cabbage, grape and banana by QuEChERS/HPLC-MS/MS[J]. J Instrum Anal, 2015, 34(5): 502
[15] 黄何何, 张缙, 徐敦明, 等. QuEChERS-高效液相色谱-串联质谱法同时测定水果中21 种植物生长调节剂的残留量[J]. 色谱, 2014, 32(7): 707
HUANG HH, ZHANG J, XU DM, et al. Simultaneous determination of 21 plant growth regulators residues in fruits by QuEChERS-highperformance liquid chromatography-tandem mass spectrometry[J]. Chin J Chromatogr, 2014, 32(7): 707
[16] 王菲, 李彤, 马辰. 超高效液相色谱-串联质谱法测定中药材中三唑类杀菌剂及三嗪类除草剂的残留量[J]. 色谱, 2013, 31(3): 191
WANG F, LI T, MA C. Determination of triazole fungicides and triazine herbicides residues in traditional Chinese medicines by high-performance liquid chromatography-tandem mass spectrometry[J]. Chin J Chromatogr, 2013, 31(3): 191
[17] 李纯, 熊颖, 顾利红, 等. 广陈皮中71 种禁限用农药残留测定分析[J]. 药物分析杂志, 2020, 40(5): 843
LI C, XIONG Y, GU LH, et al. Determination and analysis of 71 prohibited and restricted pesticides residues in pericarpium CITRI reticulatae[J]. Chin J Pharm Anal, 2020, 40(5): 843
[18] PUCCI V, PALMA S D, ALFIERI A, et al. A novel strategy for reducing phospholipids-based matrix effect in LC-ESI-MS bioanalysis by means of hybrid-SPE[J]. J Pharm Biomed Anal, 2009, 50(5): 867
[19] KMELLÁR B, FODOR P, PAREJA L, et al. Validation and uncertainty study of a comprehensive list of 160 pesticide residues in multi-class vegetables by liquid chromatography-tandem mass spectrometry[J]. J Chromatogr A, 2008, 1215(1/2): 37
