College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.
Anal Chim Acta. 2013 Jun 5;781:63-71. doi: 10.1016/j.aca.2013.04.027. Epub 2013 Apr 25.
A selective and sensitive isotope dilution-high performance liquid chromatography-linear ion trap mass spectrometry (Isotope Dilution-HPLC-LIT-MS(3)) method was developed for the simultaneous determination of 19 triazine pesticides and their degradation products in processed cereal samples from Chinese total diet study (TDS). The method integrated the addition of isotope internal standards, liquid-liquid extraction (LLE), clean-up with MCX solid-phase extraction (SPE) cartridges and HPLC-LIT-MS(3) analysis with selected reaction monitoring (SRM) mode. Matrix-matched calibration curves showed good linearity (R(2)≥0.9940) verified by applying the Mandel's fitting test (p>0.087) performed at the 95% confidence level. Decision limits (CCαs) and detection capabilities (CCβs) of the 19 triazine pesticides and their degradation products fell in the ranges of 0.0020-0.4200 μg kg(-1) and 0.0024-0.4500 μg kg(-1), respectively. Recoveries ranged from 70.1% to 112.8%, with the relative standard deviations (RSDs) ranging from 1.5% to 13.5%. Furthermore, the proposed method was applied to analyzing the proposed cereal samples from the fourth Chinese TDS. Eleven triazines were detected in six cereal samples with the concentrations ranging from 0.013 to 0.987 μg kg(-1). This method can also be used for the further determination of the triazines in other food group composites, and ultimately served as a methodological foundation for assessing the triazines in the average Chinese diet in the general population.
建立了一种用于同时测定中国总膳食研究(TDS)加工谷类样品中 19 种三嗪类农药及其降解产物的同位素稀释-高效液相色谱-线性离子阱质谱(Isotope Dilution-HPLC-LIT-MS(3))方法。该方法集成了添加同位素内标物、液液萃取(LLE)、MCX 固相萃取(SPE)小柱净化和 HPLC-LIT-MS(3)分析(采用选择反应监测(SRM)模式)。基质匹配校准曲线在 95%置信水平下通过应用 Mandel 拟合检验(p>0.087)显示出良好的线性(R(2)≥0.9940)。19 种三嗪类农药及其降解产物的决策限(CCαs)和检测能力(CCβs)分别在 0.0020-0.4200 μg kg(-1)和 0.0024-0.4500 μg kg(-1)范围内。回收率为 70.1%-112.8%,相对标准偏差(RSDs)为 1.5%-13.5%。此外,该方法还应用于分析第四次中国 TDS 中的建议谷类样品。在六个谷类样品中检测到 11 种三嗪,浓度范围为 0.013-0.987 μg kg(-1)。该方法还可用于进一步测定其他食物组混合物中的三嗪,最终为评估一般人群中普通中国人饮食中的三嗪提供了方法学基础。