色谱

色谱 ›› 2013, Vol. 31 ›› Issue (10): 980-988.DOI: 10.3724/SP.J.1123.2013.04043

• 研究论文 • 上一篇    下一篇

河水中兽药多残留分析时亲水亲脂平衡柱的基质效应和保留效果

林姗姗, 易启同, 洪家俊, 陈猛, 袁东星   

  1. 福建省海陆界面生态环境重点实验室, 厦门大学环境与生态学院, 福建 厦门 361005
  • 收稿日期:2013-04-24 修回日期:2013-05-27 出版日期:2013-10-28 发布日期:2013-10-08
  • 通讯作者: 陈猛
  • 基金资助:

    福建省自然科学基金项目(2012J01048);中国科学院城市环境研究所开放基金项目(KLUEH201009).

Matrix effect and retention efficiency of hydrophilic-lipophilic balance cartridges in multi-residual determination of veterinary drugs in river water

LIN Shanshan, YI Qitong, HONG Jiajun, CHEN Meng, YUAN Dongxing   

  1. Fujian Provincial Key Laboratory for Coastal Ecology and Environmental Studies, College of the Environment and Ecology, Xiamen University, Xiamen 361005, China
  • Received:2013-04-24 Revised:2013-05-27 Online:2013-10-28 Published:2013-10-08

PDF

212

被引次数

4

摘要：

基质效应是液相色谱-质谱联用(LC-MS)定量分析中的重要干扰因素。以反渗透水为空白对照进行LC-MS/MS检测,在500倍浓缩条件下考察了33种兽药分别经Waters、Supelco和CNW等3种亲水亲脂平衡(hydrophilic-lipophilic balance, HLB)固相萃取柱富集后的基质效应及其保留效果。结果表明,以反渗透水为基质时3种HLB柱均表现出外源性基质效应,对大部分喹诺酮类和四环素类兽药呈现促进效应,有两种HLB柱对雌激素类兽药等呈现抑制效应,对磺胺类兽药的基质效应不显著,有一种HLB柱对氯霉素类兽药呈现抑制效应;以河水为基质时,由于外源性杂质与内源性杂质共同作用,对大部分喹诺酮类和四环素类兽药呈现促进效应,对氯霉素类和雌激素类兽药呈现抑制效应,对磺胺类兽药基质效应不显著。与外标法相比较,基质匹配标准校正法可有效消除基质效应对检测结果的影响。在50 ng/L和200 ng/L两个加标水平下,Waters、Supelco和CNW 3种HLB柱对河水中33种目标兽药的校正后的回收率分别为40.3%~146.0%、37.8%~104.2%和52.9%~150.1%; RSD(n=4)为0.2%~14.6%。相同实验条件下3种HLB柱的外源性基质效应不容忽视。而采用基质匹配标准校正法克服目标物基质效应,保留效果无显著差异,富集效果良好,为河水样品中兽药多残留分析方法中固相萃取柱的选择提供了科学依据。

关键词: 保留效果, 河水, 基质效应, 亲水亲脂平衡柱, 兽药, 液相色谱-质谱

Abstract:

Matrix effect is an important interfering factor in LC-MS quantitative analysis. In this paper, matrix effects and retention efficiencies of 33 veterinary drugs spiked in river water were studied on hydrophilic-lipophilic balance (HLB) cartridges of 3 brands (Waters, Supelco, and CNW), using LC-MS/MS for detection and reverse osmosis (RO) water as the control under 500-fold concentration. In RO water, only the exogenous matrix effects were observed on three brands of HLB cartridges. Most quinolones and tetracyclines showed positive matrix effects. Estrogens showed negative matrix effects on two brands of HLB cartridges. Sulfonamides were not obviously affected by matrix effects. Chloramphenicols showed negative matrix effects on one brand of HLB cartridge. In river water, matrix effects were different from those of the RO water due to the combined exogenous and endogenous interfering substances. Sulfonamides showed slight matrix effects as those in RO water. Most quinolones and tetracyclines showed positive matrix effects. Chloramphenicols and estrogens showed negative matrix effects. Compared to the external standard method, matrix matched calibration method effectively overcame the matrix effects with better quantitative results. The recoveries of 33 target veterinary drugs spiked in river water at 50 ng/L and 200 ng/L levels were in the ranges of 40.3%-146.0% (Waters), 37.8%-104.2% (Supelco), and 52.9%-150.1% (CNW) with RSDs (n=4) of 0.2%-14.6%. The results indicated that there was no significant difference in the retention efficiency between the 3 HLB cartridges with the matrix matched calibration method. This study provided supporting data for the HLB cartridge selection in multi-residual determination of the veterinary drugs in river water samples.

Key words: hydrophilic-lipophilic balance (HLB) cartridges, liquid chromatography-mass spectrometry, matrix effect, retention efficiency, river water, veterinary drug

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