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Multiresidue GC-MS/MS pesticide analysis for evaluation of tea and herbal infusion safety

机译:多残留GC-MS / MS农药分析用于评估茶和草药的安全性

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摘要

A fast, simple, low-cost and high-throughput multiresidue pesticide analysis method was developed and validated for 300 pesticides in herbal and fruit infusion samples based on modified QuEChERS (quick, easy, cheap, effective, rugged and safe) procedure combined with gas chromatography coupled with tandem mass spectrometry method (GC-MS/MS). The objectives were to develop low cost GC-MS/MS method, validate the method in accordance to SANTE/11,813/2017 guidance document and application in routine. The results obtained using different GC and MS/MS parameters were evaluated in order to develop quick, robust, accurate and effective multiresidue method. Total analysis time was 28min with 0.6 mu L injection volume. For accurate quantification, matrix-matched calibration (MMC) curves (in range of 10 mu g/kg - 250 mu g/kg) were applied to compensate matrix effect. The limits of quantification (LOQ) were ranged between 0.06 mu g/kg and 135 mu g/kg, and for the majority of the pesticides the LOQ were below the regulatory maximum residue limits. Most recoveries at 10 mu g/kg and 100 mu g/kg were in the range 70%-120% indicating satisfactory accuracy. The validated method was applied to commercial herbal and fruit infusion products detecting chlorpyriphos, DEET, tebuconazole, terbuthylazine, piperonyl butoxide, biphenyl, pendimethalin, pirimiphos-methyl and p,p'-DDE in more than 100 samples from 1,466 so risk assessment on human health was calculated specially for those pesticides.
机译:开发了一种快速,简单,低成本,高通量的多残留农药分析方法,并基于改良的QuEChERS(快速,简便,廉价,有效,坚固和安全)程序结合气体对草药和水果注入样品中的300种农药进行了验证色谱-串联质谱联用(GC-MS / MS)。目标是开发低成本的GC-MS / MS方法,根据SANTE / 11,813 / 2017指导文件验证该方法并在常规中应用。评估了使用不同GC和MS / MS参数获得的结果,以开发快速,可靠,准确和有效的多残留方法。进样量为0.6μL的总分析时间为28分钟。为了精确定量,应用了基质匹配校准(MMC)曲线(范围为10μg/ kg-250μg/ kg)来补偿基质效应。定量限(LOQ)介于0.06μg/ kg和135μg/ kg之间,对于大多数农药,LOQ均低于规定的最大残留限量。在10μg / kg和100μg / kg的情况下,大多数回收率在70%-120%的范围内,表明令人满意的准确性。经验证的方法已用于商业草药和水果浸泡产品,从1,466份样品中检测了100多个样品中的毒死,、 DEET,戊唑醇,丁噻嗪,胡椒基丁醚,联苯,二甲戊灵,对苯二甲酰甲基和p,p'-DDE。健康是专门针对那些农药计算的。

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