UPLC-MS/MS法测定白术中8种植物生长调节剂残留量及风险评估

Determination of Eight Plant Growth Regulators Residues in Atractylodes macrocephala Rhizoma by UPLC-MS/MS Method and Risk Assessment

关键词:  白术  植物生长调节剂  超高效液相色谱-串联质谱法  膳食摄入风险评估

Key words:  Atractylodes macrocephala Rhizoma  plant growth regulators  ultra-performance liquid chromatography-tandem mass spectrometry  dietary intake risk assessment

摘要:

目的 采用超高效液相色谱串联质谱法（UPLC-MS/MS），建立白术中8种植物生长调节剂（PGRs）的测定方法，制定相关生长调节剂的限量标准，并进行初步的风险评估。方法 采用乙腈-0.01%甲酸水溶液为流动相梯度洗脱，正负离子切换多反应监测模式，并进行方法学验证。结合国内外相关的食品和中药材标准，通过慢性摄入风险评估（HQc）和急性摄入风险评估（HQa）对PGRs残留风险进行评价。结果 8种植物生长调节剂在相应的测定范围内线性关系良好，相关系数均大于0.995，三个添加水平回收率均在91%~140%之间。30 批白术中共检出7 种植物生长调节剂，总检出率为76.67%，风险分析得出HQc和HQa均小于1，表明白术中PGRs的膳食暴露风险处于较低水平。结论 该方法灵敏度高，准确性好，且前处理简单快速，可用于白术中植物生长调节剂的残留量测定。虽然白术中植物生长调节剂残留风险较低，但由于其在中药中的长期累积效应，低剂量暴露仍可能会对人体健康产生潜在影响，当前仍需加强监管，建议制定定量限标准以规范种植和生产，确保药材安全性和有效性。

Abstract:

OBJECTIVE To establish an ultra-performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) method for determining eight plant growth regulators (PGRs) in Atractylodis Macrocephalae Rhizoma, establishment of corresponding maximum residue limits, and conduct preliminary risk assessment. METHODS Chromatographic separation utilized acetonitrile-0.01% formic acid mobile phase under gradient elution, with MRM detection via polarity switching, followed by method validation. PGRs residue risks were assessed through HQc and HQa, referencing domestic and international standards for food and medicinal herbs. RESULTS? All eight plant growth regulators exhibited satisfactory linearity within their respective detection ranges, with correlation coefficients exceeding 0.995. Mean recoveries across three fortification levels ranged from 91% to 140%. Analysis of thirty Atractylodis Macrocephalae Rhizoma?batches detected seven PGRs, showing an overall detection frequency of 76.67%. Risk assessment determined both HQc and HQa values below 1, indicating low dietary exposure risks associated with PGR residues in this medicinal material. CONCLUSION ?This method demonstrates high sensitivity, good accuracy, and simple and rapid sample preparation, making it suitable for determining PGR residues in Atractylodis Macrocephalae Rhizoma?rhizomes. Although PGR residues in?Atractylodis Macrocephalae Rhizoma?pose acceptable risk levels, long-term use in TCM may still pose health risks due to accumulated low-dose exposure, enhanced regulatory oversight is recommended. Establishing residue limit standards would standardize cultivation and production practices, ensuring the safety and efficacy of this medicinal material.