Validation of a high-throughput method for analysis of pesticide residues in hemp and hemp products
Validation of a high-throughput method for analysis of pesticide residues in hemp and hemp products
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DOI：
10.1016/j.chroma.2021.462097
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发表时间：
2021-04-10
影响因子：
4.1
通讯作者：
Repetti, Maria Rosa
中科院分区：
文献类型：
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作者：
Michlig, Nicolas;Lehotay, Steven J.;Repetti, Maria Rosa
几千年来，大麻一直是一种农产品，由于其大麻素、蛋白质、纤维和其他成分含量高，人们对大麻的兴趣和产量一直在复苏。为了在美国境内合法拥有和使用，大麻和大麻产品的 delta-9-四氢大麻酚 (THC) 浓度必须 < 0.3%。与大多数作物一样，种植大麻时可能会使用农药，这需要在食品、饲料和药品中进行监测。这项工作的目的是评估和验证最近开发的“快速、简单、廉价、有效、坚固、安全、高效和稳健”(QuEChERSER) 样品制备大方法，用于测定大麻植物、花朵、粉末、油和颗粒中的农药残留。对北美监测清单中 106 种目标农药和代谢物的最终提取物进行高通量分析需要：1) 超高效液相色谱-串联质谱 (UHPLC-MS/MS)，带柱反冲洗，2) 仪器顶部样品制备 + 低压气相色谱 (ITSP+LPGC-MS/MS)。在 QuEChERSER 中，用 10 mL 4/1 (v/v) 乙腈/水机械摇动 10 分钟提取 2 g 样品，然后离心 3 分钟。对于 LC，取 0.2 mL 提取物并将溶剂更换为初始流动相，然后进行 5 分钟超速离心，然后进行 10 分钟分析。对于适合 GC 的农药，将剩余的初始提取物用 4/1 (w/w) anh 分配。 MgSO4/NaCl，并取 1 mL 用于自动 ITSP 净化，同时进行 10 分钟 LPGC 分析。在前一种情况下，UHPLC 柱在每次进样之间用 1/1 (v/v) 甲醇/乙腈反冲洗 3 分钟，以保持系统清洁并避免鬼峰。多层次、多天的验证结果实现了 70-120% 的回收率，大麻蛋白粉、油、颗粒和新鲜植物（干大麻植物和花过于复杂）中超过 80% 的分析物的 RSD < 20%。几乎所有农药的定量限 (LOQ) 均小于 10 ng/g，加标样品中超过 13,000 个分析物结果中出现 2.8% 的假阴性。 QuEChERSER 方法被证明可以应对几种复杂大麻基质的挑战。由 Elsevier B.V. 出版
Hemp has been an agricultural commodity for millennia, and it has been undergoing a resurgence in interest and production due to its high content of cannabinoids, protein, fiber and other ingredients. For legal possession and use throughout the USA, hemp and hemp products must have delta-9-tetrahydrocannabinol (THC) concentration < 0.3%. As with most crops, pesticides may be applied when farming hemp, which need to be monitored in food, feed, and medicinal products. The aim of this work was to evaluate and validate the recently developed "quick, easy, cheap, effective, rugged, safe, efficient, and robust" (QuEChERSER) sample preparation mega-method to determine pesticide residues in hemp plants, flowers, powders, oils, and pellets. High-throughput analysis of final extracts for 106 targeted pesticides and metabolites from North American monitoring lists entailed: 1) ultrahigh-performance liquid chromatography - tandem mass spectrometry (UHPLC-MS/MS) with column back-flushing, and 2) instrument-top sample preparation + low-pressure gas chromatography (ITSP+LPGC-MS/MS). In QuEChERSER, 2 g sample is extracted with 10 mL 4/1 (v/v) acetonitrile/water by mechanical shaking for 10 min, followed by 3 min centrifugation. For LC, 0.2 mL of extract is taken and solvent exchanged into initial mobile phase followed by 5 min ultra-centrifugation prior to the 10 min analysis. For GC-amenable pesticides, the remaining initial extract is partitioned with 4/1 (w/w) anh. MgSO4/NaCl, and 1 mL is taken for automated ITSP cleanup in parallel with 10 min LPGC analysis. In the former case, the UHPLC column is back-flushed with 1/1 (v/v) methanol/acetonitrile for 3 min between each injection to keep the system clean and avoid ghost peaks. Multi-level, multi-day validation results achieved 70-120% recoveries with RSDs < 20% for more than 80% of the analytes in hemp protein powder, oil, pellets, and fresh plant (dried hemp plant and flower were too complex). Limits of quantification (LOQs) were < 10 ng/g were achieved for nearly all pesticides, yielding 2.8% false negatives among >13,000 analyte results in the spiked samples. The QuEChERSER method was demonstrated to meet the challenge for several complex hemp matrices. Published by Elsevier B.V.