黄瓜粉中氯吡脲残留分析标准物质研究

    Development of Certified Reference Material for Forchlorfenuron Residue in Cucumber Powder

    • 摘要: 基体标准物质(CRMs)在验证分析方法和质量控制中起着重要作用。为保证植物生长调节剂风险评估结果的准确性和可靠性,首次研制了黄瓜粉中氯吡脲标准物质,以提高黄瓜中氯吡脲残留测量质量。实验经制浆、加药、均质、冷冻干燥、研磨、筛分、混合、包封等工序制备了标准物质候选物;优化并建立了液相色谱-串联同位素稀释质谱法(ID-LC/MS/MS)定值方法,并将其用于标准物质的定值。结果表明,黄瓜粉中氯吡脲特性量值为14.7 mg/kg,扩展不确定度为2.7 mg/kg (k=2)。同时,还评估了特性量的均匀性,以及在−20℃下9个月的长期稳定性和40℃条件下9天的短期稳定性,并全面分析与评估了定值、均匀性和稳定性的引入的不确定度。

       

      Abstract: Matrix certified reference materials (CRMs) play a crucial role in validating analytical methods and ensuring quality control. To enhance the accuracy and reliability of risk assessments for plant growth regulators, we have developed a certified reference material (CRM) for forchlorfenuron in cucumber powder, thereby improving the measurement quality of forchlorfenuron residues in cucumbers. The CRM was prepared through processes including pulping, drug-adding, homogenization, freeze-drying, grinding, sieving, mixing, and encapsulation. The liquid chromatography-tandem isotope dilution mass spectrometry (ID-LC/MS/MS) method was optimized and established for the quantification of the CRM. The certified value of forchlorfenuron in cucumber powder was determined to be 14.7 mg/kg with an expanded uncertainty of 2.7 mg/kg (k=2). Furthermore, the homogeneity of the material was assessed, along with its long-term stability at −20°C over nine months and short-term stability at 40°C over nine days. The study comprehensively evaluated uncertainties introduced by characterization, homogeneity, and stability assessments.

       

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