固相萃取净化-高效液相色谱法测定肉制品中的9 种N-亚硝基化合物

建立采用固相萃取-高效液相色谱法同时测定肉制品中9 种N-亚硝基化合物的方法。以甲醇为提取剂，60 ℃条件下超声提取，经CNWBOND HC-C18固相萃取柱净化后，采用AQ-C18色谱柱分析。甲醇和超纯水为流动相实现了待测物的良好分离，紫外检测器检测，结合保留时间和光谱图定性，外标法定量。结果表明：9 种N-亚硝基化合物线性关系良好，相关系数均大于0.99；方法定量限（RSN = 10）为0.047～0.097 μg/g；回收率为72.6%～97.6%；相对标准偏差（n＝6）为3.1%～7.9%。此方法前处理简单、回收率高、精密度好，适用于肉制品中9 种N-亚硝基化合物的同时测定。

Determination of Nine N-Nitroso Compounds in Meat Products by Solid Phase Extraction Purification and High Performance Liquid Chromatography

A solid-phase extraction (SPE)-high performance liquid chromatography (HPLC) method has been developed forsimultaneous determination of 9 N-nitroso compounds (NOCs) in meat products. The analytes were extracted with methanolat 60 ℃ ultrasonically, purified by a CNWBOND HC-C18 SPE column, and analyzed by HPLC on a Phenomenex AQ-C18column (250 mm × 4.6 mm, 5 μm) employing methanol and ultrapure water as the mobile phase in a gradient elution mode.The 9 N-nitroso compounds were qualitatively determined by retention time, and confirmed by ultraviolet spectroscopy.The results indicated that the calibration curves of the target analytes displayed good linearity with correlation coefficients(r) greater than 0.99. The method limits of quantification (MLOQ) for the target analytes ranged from 0.047 to 0.097 μg/g(RSN =10). The recoveries were in the range between 72.6% and 97.6%, and the precision (relative standard deviation, RSD)ranged from 3.1% to 7.9% (n = 6).