UHPLC-MS/MS Determination of Residual Amounts of Citrinin, Alternariol and Alternariolmethylether in Grapes
摘 要
采用超高效液相色谱-串联质谱法测定葡萄中桔青霉素、链格孢酚和链格孢酚甲基乙醚的残留量。葡萄样品经乙腈提取,氯化钠和无水硫酸镁除水,C18粉末净化除杂,有机滤膜过滤。以ACQUITY UPLC BEH C18色谱柱为分离柱,以不同体积比的乙腈和5 mmol·L-1乙酸铵溶液的混合液为流动相进行梯度洗脱,采用电喷雾正、负离子源多反应监测模式检测。3种化合物的质量浓度均在5~100 μg·L-1内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为0.3~0.6 μg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为79.0%~97.0%,测定值的相对标准偏差(n=5)为0.80%~5.2%。
Abstract
UHPLC-MS/MS was applied to the determination of residual amounts of citrinin, alternariol and alternariolmethylether in grapes. Grape sample was extracted with acetonitrile, and then NaCl and anhydrous magnesium sulfate were used to remove the water. C18 powder was added for purification in addition to miscellaneous, and organic membrane was used to filter. ACQUITY UPLC BEH C18 chromatographic column was used as stationary phase, and the mixtures of acetonitrile and 5 mmol·L-1 ammonium acetate solution mixed in different ratios were used as mobile phase in gradient elution. ESI+, ESI- and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 3 compounds were kept in the same range of 5-100 μg·L-1, with detection limits (3S/N) in the range of 0.3-0.6 μg·kg-1. On the base of blank sample, test for recovery was made by standard addition method. Values of recovery found were in the range of 79.0%-97.0%, with RSD's (n=5) in the range of 0.80%-5.2%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201802010
所属栏目 工作简报
基金项目 国家农产品质量安全监管(风险评估)(GJFP2017004,GJFP2017011,GJFP2017015);中国热带农业科学院基本科研业务费专项资金(1630122017020);海南省自然科学基金(0110200027)
收稿日期 2017/2/20
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备注林玲(1978-),女,海南海口人,副研究员,硕士,主要从事农药、兽药残留检测技术研究工作
引用该论文: LIN Ling,LIU Yuanjing,CHA Yubing,GUO Hongbin,ZHANG Liqiang,YANG Chunliang. UHPLC-MS/MS Determination of Residual Amounts of Citrinin, Alternariol and Alternariolmethylether in Grapes[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(2): 172~176
林玲,刘元靖,查玉兵,郭宏斌,张利强,杨春亮. 超高效液相色谱-串联质谱法测定葡萄中桔青霉素、链格孢酚和链格孢酚甲基乙醚的残留量[J]. 理化检验-化学分册, 2018, 54(2): 172~176
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【3】杨欣.链格孢霉毒素研究进展[J].国外医学卫生学分册, 2000,27(3):182-187.
【4】李燕,仇峰,杨美华,等.高效液相色谱-串联质谱法测定中药中桔青霉素[J].药物分析杂志, 2011,31(9):1726-1730.
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【6】胡媛媛,马良,张宇昊.柑橘果实中主要的真菌毒素及其检测技术[J].食品工业科技, 2013,34(24):385-390.
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【8】陈蕴,许赣荣,顾玉梅,等.TLC及HPLC测定红曲产品中的桔霉素[J].无锡轻工大学学报, 2001,20(2):164-168.
【9】陈军,李章万,祁伟,等.RP-HPLC测定红曲中的桔青霉素[J].华西药学杂志, 2008,23(2):219-221.
【10】DELGADO T, GOMEZ CORDOVES C. Natural occurrence of alternariol and alternariol methylether in Spanish apple juice concentrates[J]. Chromatography A, 1998,815(1):93-97.
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