高效液相色谱-串联质谱法快速测定短货架期水果中11种防腐剂含量

Rapid determination of 11 kinds of preservatives content in short-shelf-life fruits by high performance liquid chromatography-tandem mass spectrometry

中文关键词:  新鲜水果，高效液相色谱-串联质谱法，QuEChERS，防腐剂

英文关键词:short-shelf-life fruits  high performance liquid chromatography-tandem mass spectrometry  QuEChERS  preservatives

中文摘要:

      目的 建立QuEChERS结合高效液相色谱-串联质谱法检测短货架期水果中11种防腐剂含量的分析方法。方法 样品经甲醇提取后, 吸取2.0 mL提取液加入100 mg N-丙基乙二胺(N-primary secondary amine, PSA)、100 mg球形十八烷基硅烷(C18)粉末净化管, 涡旋混匀1 min后, 4500 r/min离心5 min, 取上清液过0.22 μm有机微孔滤膜后, 使用电喷雾正、负离子模式, 以多反应监测模式采集。结果 11种防腐剂线性范围内具有良好的线性关系, 相关系数(r)均大于0.99, 检出限为0.003~0.015 mg/kg, 定量限为0.01~0.05 mg/kg, 在杨梅、桑葚、草莓基质中添加3个不同质量浓度的防腐剂, 平均加标回收率为76.4%~98.9%, 相对标准偏差(relative standard deviations, RSDs)为0.5%~9.8%。将方法用于20批次杨梅、桑葚、草莓样品中防腐剂的分析, 发现2批桑葚、1批次杨梅中检出纳他霉素检出, 含量范围为4.5~11.9 mg/kg。结论 该方法操作简单, 灵敏度高, 可实现多种防腐剂的快速测定, 为短货架期水果中多种防腐剂同时监测、评估提供技术支撑。

英文摘要:

      Objective To establish an analytical method for the detection of 11 kinds of preservatives content in short-shelf-life fruits by QuEChERS combined with high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with methanol, and 2.0 mL of the extract was transferred to a purification tube containing 100 mg of N-primary secondary amine (PSA) and 100 mg of C18 powder. After vortex mixing for 1 min and centrifugation at 4500 r/min for 5 min, the supernatant was passed through a 0.22 μm organic microporous membrane. The sample was analyzed in multiple reaction monitoring mode using electrospray negative and postive ionization mode. Results The results demonstrated good linearity for all 11 kinds of preservatives within their respective concentration ranges, with correlation coefficients (r) exceeding 0.99. The method exhibited limits of detection of 0.003–0.015 mg/kg and limits of quantitation of 0.01–0.05 mg/kg. For recovery studies in bayberry, mulberry and strawberry matrices at 3 spiked mass concentration levels, the average recoveries ranged from 76.4% to 98.9%, with relative standard deviations (RSDs) of 0.5%–9.8%. When applied to 20 batches of bayberry, mulberry and strawberry samples, natamycin was detected in 2 batches of mulberries and one batch of bayberries, with concentrations ranging from 4.5 to 11.9 mg/kg. Conclusion The method is simple, highly sensitive, and enables rapid determination of multiple preservatives, providing technical support for the simultaneous monitoring and evaluation of various preservatives in short-shelf-life fruits.