作者：贺光云1,2, 韩梅1,2, 邱世婷1,2, 吴亚姗3, 李莹1,2, 覃蜀迪1,2, 夏斯琪1,2, 陈思宇4, 侯雪1,2, 付才力4
作者单位：1. 四川省农业科学院农业质量标准与检测技术研究所, 四川 成都 610066;
2. 农业农村部农产品质量安全风险评估实验室(成都), 四川 成都 610066;
3. 四川省农产品质量安全中心, 四川 成都 610041;
4. 新加坡国立大学苏州研究院, 江苏 苏州 215000
关键词：辣椒粉;直接稀释法;UPLC-QTOF-MS;合成染料;快速检测
摘要：
采用直接稀释前处理法，结合超高效液相色谱-四极杆串联飞行时间质谱（UPLC-QTOF-MS），对辣椒粉中苏丹红等20种禁用合成染料进行快速分析。该方法以水/乙腈/丙酮（v/v/v=2/3/3）混合体系为提取溶剂，提取液未经净化，用0.1%甲酸甲醇溶液稀释5倍后进行UPLC-QTOF-MS分析，在8 min内实现20种染料的良好分离及检测，定量限（LOQ）为1~40 μg/kg，回收率为54.72%~117.77%，RSD在0.56%~16.27%范围，满足检测要求。将建立的方法应用于30个辣椒粉样品中目标染料的检测，未检出阳性样品。该方法样品前处理过程快速简化，节约溶剂、降低检测成本、缩短分析周期，符合绿色检验检测要求。
Rapid determination of twenty synthetic dyes in chilli powders by a dilute-and-shoot approach coupled with UPLC-QTOF-MS
HE Guangyun, HAN Mei, QIU Shiting, WU Yashan, LI Ying, QIN Shudi, XIA Siqi, CHEN Siyu, HOU Xue, FU Caili
1. Institute of Quality Standard and Testing Technology for Agro-Products, Sichuan Academy of Agricultural Sciences, Chengdu 610066, China;
2. Laboratory of Quality and Safety Risk Assessment for Agro-Products (Chengdu), Ministry of Agriculture and Rural Affair, Chengdu 610066, China;
3. Sichuan Agricultural Products Quality and Safety Center, Chengdu 610041, China;
4. NUS (Suzhou) Research Institute, Suzhou 215000, China
Abstract: A dilute-and-shoot based ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry (UPLC-QTOF-MS) method was developed for rapid analysis of 20 fat-soluble synthetic dyes in chilli powders. The target synthetic dyes including Sudan dyes were extracted with water/acetonitrile/acetone (v/v/v=2/3/3), followed by a 5-fold dilution with methanol containing 0.1% formic acid before UPLC-QTOF-MS analysis. The pretreatment and analysis conditions were optimized in the process. The optimized method facilitated the separation and detection of the twenty dyes within 8 min, and indicated good sensitivity with LOQ of 1-40 μg/kg. Recovery rates ranged between 54.72% and 117.77% for all the analytes with RSDs of 0.56%-16.27%. The developed method was applied for the detection of the target dyes in 30 chilli powder samples and all the samples were tested negative. Allowing the determination of the target dyes with the advantages of simple pretreatment, short extraction time, as well as being solvent-saving and easy to operate, the dilute-and-shoot procedure meets the requirements of green analysis.
Keywords: chilli powder;dilute-and-shoot;UPLC-QTOF-MS;synthetic dye;rapid determination
2023, 49(11):110-118 收稿日期: 2022-05-12;收到修改稿日期: 2022-07-25
基金项目: 四川省杰出青年科技人才项目（2020JDJQ0072）；福州市科技特派员后补助项目（AFZ2021K010003）；江苏如皋市科技攻关计划项目（SRG(21)1040）
作者简介: 贺光云(1980-),女,云南镇雄县人,副研究员,博士,主要从事农产品质量安全风险评估研究。
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