这项研究证明了自动化的高通量迷你柱式固相萃取(mini-SPE)净化技术在快速低压气相色谱-串联质谱(LPGC-MS/MS)分析农药和环境污染物中的应用食品的QuEChERS提取物。使用鳄梨比较了使用不同迷你SPE吸附剂的净化效率和突破体积,鲑鱼,猪腰,和羽衣甘蓝作为代表矩阵。对于含有20/12/12/1(w/w/w/w)anh的45mg微型药筒,最佳提取物负载体积为300µL。在最终方法中使用的MgSO4/PSA(伯仲胺)/C18/CarbonX吸附剂。在方法验证中,展示高吞吐量能力和性能结果,10种不同食物的230种加标提取物(苹果,猕猴桃,胡萝卜,羽衣甘蓝,橙色,黑橄榄,小麦谷物,干罗勒,猪肉,和鲑鱼)在5天内进行了自动迷你SPE清理和分析。总之,使用10分钟LPGC-MS/MS方法对54种农药和43种环境污染物进行了325次分析(一起分析了3种),而无需更换衬里或重新调整仪器。仅仅,注射的1mg等效样品达到<5ngg-1的定量限。随着内部标准的使用,方法验证结果表明,在10种测试食品基质(n=160)中,94种分析物对中的91种获得了令人满意的结果(回收率为70-120%,RSD≤25%)。基体效应通常小于±20%,主要是由于使用了分析物保护剂,由于分析物峰的求和函数积分,因此需要对软件数据处理进行最少的人工审查。这项研究表明,自动化的mini-SPE+LPGC-MS/MS方法在粗糙的情况下产生了准确的结果,以最少的人工和数据审查进行高通量操作。
This study demonstrated the application of an automated high-throughput mini-cartridge solid-phase extraction (mini-SPE) cleanup for the rapid low-pressure gas chromatography-tandem mass spectrometry (LPGC-MS/MS) analysis of pesticides and environmental contaminants in QuEChERS extracts of foods. Cleanup efficiencies and breakthrough volumes using different mini-SPE sorbents were compared using avocado, salmon, pork loin, and kale as representative matrices. Optimum extract load volume was 300 µL for the 45 mg mini-cartridges containing 20/12/12/1 (w/w/w/w) anh. MgSO4/PSA (primary secondary amine)/C18/CarbonX sorbents used in the final method. In method validation to demonstrate high-throughput capabilities and performance results, 230 spiked extracts of 10 different foods (apple, kiwi, carrot, kale, orange, black olive, wheat grain, dried basil, pork, and salmon) underwent automated mini-SPE cleanup and analysis over the course of 5 days. In all, 325 analyses for 54 pesticides and 43 environmental contaminants (3 analyzed together) were conducted using the 10 min LPGC-MS/MS method without changing the liner or retuning the instrument. Merely, 1 mg equivalent sample injected achieved <5 ng g-1 limits of quantification. With the use of internal standards, method validation results showed that 91 of the 94 analytes including pairs achieved satisfactory results (70-120 % recovery and RSD ≤ 25 %) in the 10 tested food matrices (n = 160). Matrix effects were typically less than ±20 %, mainly due to the use of analyte protectants, and minimal human review of software data processing was needed due to summation function integration of analyte peaks. This study demonstrated that the automated mini-SPE + LPGC-MS/MS method yielded accurate results in rugged, high-throughput operations with minimal labor and data review.