食品科学 ›› 2020, Vol. 41 ›› Issue (4): 319-324.doi: 10.7506/spkx1002-6630-20190410-137

• 安全检测 • 上一篇    

超高效液相色谱-串联质谱法同时测定水果中10 种保鲜剂残留量

曹雪琴,杨飞,陈国通,毛琼玲,李芳,杨中   

  1. (1.新疆维吾尔自治区分析测试研究院,新疆 乌鲁木齐 830011;2.中国科学院新疆理化技术研究所,新疆 乌鲁木齐 830011)
  • 收稿日期:2020-03-02 修回日期:2020-03-02 出版日期:2020-02-25 发布日期:2020-03-02

Determination of 10 Preservative Residues in Fruits by Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

CAO Xueqin, YANG Fei, CHEN Guotong, MAO Qiongling, LI Fang, YANG Zhong   

  1. (1. Xinjiang Academy of Analysis and Testing, ürümqi 830011, China; 2. Xinjiang Technical Institute of Physics and Chemistry, Chinese Academy of Sciences, ürümqi 830011, China)
  • Received:2020-03-02 Revised:2020-03-02 Online:2020-02-25 Published:2020-03-02

摘要: 建立超高效液相色谱-串联质谱法同时测定水果中咪鲜胺、多菌灵、甲基硫菌灵、噻菌灵、异菌脲、抑霉唑、苯菌灵、腐霉利、百菌清、嘧霉胺10 种保鲜剂残留方法。样品用QuEChERS方法处理,经Acquity UPLC BEH C18色谱柱分离,乙腈-0.1%甲酸溶液为流动相梯度洗脱,经超高效液相色谱-串联质谱仪采用电喷雾电离源多反应监测模式检测,基质匹配标准溶液外标法定量。结果表明,10 种保鲜剂在各自质量浓度范围内线性良好(r>0.992),在3 个加标水平下,回收率为75.0%~112%,相对标准偏差(n=6)不大于9.5%。10 种防腐保鲜剂的检出限(RSN≥3)为0.02~1.50 μg/kg,定量限(RSN≥10)为0.1~4.1 μg/kg。该方法操作简便,灵敏度高,准确可靠,适用于水果中10 种保鲜剂残留量的同时测定。

关键词: 保鲜剂, QuEChERS, 水果, 超高效液相色谱-串联质谱法

Abstract: An analytical method for the simultaneous determination of the residues of 10 preservatives, including peimisine, carbendazim, thiophanate-methyl, thiabendazole, iprodione, imazalil, benomyl, procymidone, chlorothalonil and pyrimethanil, in fruits was developed by using ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Samples were extracted by the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. The UPLC-MS/MS method was performed with an ACQUITY UPLC BEH C18 column using gradient elution with a mobile phase of acetonitrile and 0.1% formic acid in water. The target compounds were detected by multiple reaction monitoring (MRM) with an electrospray ionization source in the positive ion mode, and quantified by an external standard method using a matrix-match standard solution. The calibration curves showed good linearity with correlation coefficients greater than 0.992. The recoveries of the 10 preservatives at three spiked levels ranged from 75.0% to 112%, with relative standard deviations (RSDs) of less than 9.5% (n = 6). The limits of detection (LODs, RSN ≥ 3) were 0.02–1.50 μg/kg and the limits of quantity (LOQs, RSN ≥ 10) were 0.1–4.1 μg/kg for all the analytes. The established method is simple, sensitive, accurate and reliable, and can be applied for the simultaneous determination of multiple preservative residues in fruits.

Key words: preservatives, QuEChERS, fruits, ultra-high performance liquid chromatography-tandem mass spectrometry

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