Determination of 4 Organophosphorous Herbicides Residues in Grape Wine by HPLC-MS/MS
摘 要
提出了同时测定葡萄酒中莎稗磷、甲基胺草磷、抑草磷和哌草磷4种有机磷类除草剂残留量的高效液相色谱-串联质谱法。样品2.000 0 g加入12 mL的乙酸乙酯和1.00 g氯化钠,涡旋混匀30 s,超声提取10 min,提取液经1.00 g PSA、0.20 g无水硫酸镁分散固相萃取净化。采用ZORBAX XDB-C18色谱柱进行分离,以体积比15∶85的0.1%(体积分数)甲酸溶液和甲醇的混合液为流动相进行等度洗脱。以电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式进行质谱分析,外标法定量。4种有机磷类除草剂的质量浓度在1.0~200.0 μg·L-1内与其峰面积呈线性关系,检出限(3S/N)为0.01~0.04 μg·kg-1。采用标准加入法在3个浓度水平上进行回收试验,回收率为69.3%~99.2%,测定值的相对标准偏差(n=5)为2.3%~8.1%。
Abstract
HPLC-MS/MS was proposed for the determination of the residual anount of 4 organophosphorus herbicides, including paspalum, methamphoron, imphoron, and piperon in grape wine. 2.000 0 g of samples were mixed with 12 mL of ethyl acetate and 1.00 g of sodium chloride by vertical oscillation for 30 s, and the solution was extracted ultrasonically for 10 min. The extract was purified with N-propyl ethylenediamine (1.00 g) and anhydrous magnesium sulfate (0.20 g) by dispersive solid phase extraction. The purified solution was then separated on ZORBAX XDB-C18 column as stationary phase and the mixture of 0.1% (φ) formic acid solution and methanol with the volume ratio of 15 to 85 was used as mobile phase in isocratic elution. ESI+ and MRM were adopted in MS analysis, and external standard method was used for quantification. Linearity relationships between values of peak area and mass concentration of 4 organophosphorus herbicides were kept in the same range of 1.0-200.0 μg·L-1, with detection limits (3S/N) in the range of 0.01-0.04 μg·kg-1. Test for recovery was made by standard addition at 3 different concentration levels, giving results in the range of 69.3%-99.2%, with RSDs of determined values (n=5) ranged from 2.3% to 8.1%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx202104010
所属栏目 工作简报
基金项目 石家庄市科学技术研究与发展指导计划(191460733);河北省医学适用技术跟踪项目(GZ2020042)
收稿日期 2020/4/21
修改稿日期
网络出版日期
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联系人作者王可(wkecdc@163.com)
备注郭爱静,主管技师,主要从事食品有机污染物分析工作
引用该论文: GUO Aijing,HUA Zhongxia,ZHANG Hong,ZHANG Shiyong,XIN Jia,WANG Ke. Determination of 4 Organophosphorous Herbicides Residues in Grape Wine by HPLC-MS/MS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2021, 57(4): 344~349
郭爱静,花中霞,张弘,张世勇,辛佳,王可. 高效液相色谱-串联质谱法测定葡萄酒中4种有机磷类除草剂残留量[J]. 理化检验-化学分册, 2021, 57(4): 344~349
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【22】郭春景,孙长华,王玉芝.快速溶剂萃取-高效液相色谱法测定莎稗磷残留[J].黑龙江农业科学, 2011(7):67-69.
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【24】KUDO K, NAGAMATSU K, UMEHARA T, et al. Rapid and reliable screening method for detection of 70 pesticides in whole blood by gas chromatography-mass spectrometry using a constructed calibration-locking database[J]. Legal Medicine, 2012,14(2):93-100.
【25】SASANO R, HAMADA T, KURANO M, et al. On-line coupling of solid-phase extraction to gas chromatography with fast solvent vaporization and concentration in an open injector liner:Analysis of pesticides in aqueous samples[J]. Journal of Chromatography A, 2000,896(1/2):41-49.
【26】郝元元.LC-MS/MS法测定柚子皮中香豆素类物质组成及含量[J].食品研究与开发, 2019,40(16):146-152.
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