Zhao Dong-Hao, Wang Qiang, Wang Xu-Feng, Li Zhi-Guang, Li Yong-Xian, Huang Ke, Li Liu-Dong
Key Lab. of Aquatic Product Processing, Ministry of Agriculture; Lab. of Quality & Safety Risk Assessment for Aquatic Product on Storage and Preservation (Guangzhou); Fishery Environment and Aquatic Products Quality Inspection & Testing Center of the Ministry of Agriculture (Guangzhou); South China Sea Fisheries Research Institute, Chinese Academy of Fishery Sciences, Haizhu District, Guangzhou, Guandong 510300, PR China.
J Chromatogr Sci. 2017 Sep 1;55(8):813-817. doi: 10.1093/chromsci/bmx041.
A practical solid-phase extraction (SPE) method coupled with liquid chromatography/tandem mass spectrometry (LC-MS/MS) has been developed for the determination of the fish anesthetic MS-222 in water. Water samples were concentrated and purified using three SPE cartridges of different specifications. Elution curves of MS-222 were constructed using various methanol-water solutions on the different cartridges, and SPE conditions were optimized in accordance with the elution curves. The mobile phase containing methanol and 0.1% formic acid solution with a linear gradient elution was utilized to separate MS-222 on a C18 column. Detection was carried out by a triple-quadrupole mass spectrometry with an electrospray ion source in positive mode. Recoveries of three MS-222 fortified levels of 0.05, 0.5 and 5 μg/L ranged of 82.6-101% with relative standard deviations (RSDs) below 9.36%. The limit of detection (LOD) and limit of quantification (LOQ) of MS-222 were 0.01 μg/L and 0.03 μg/L, respectively. This method was satisfactorily applied to the determination of MS-222 in actual water samples collected from aquatic product transportation vehicles or from the natural water catchments.
已开发出一种实用的固相萃取（SPE）方法并结合液相色谱/串联质谱（LC-MS/MS）用于测定水中的鱼类麻醉剂MS-222。使用三种不同规格的SPE小柱对水样进行浓缩和净化。在不同的小柱上使用各种甲醇-水溶液构建MS-222的洗脱曲线，并根据洗脱曲线优化SPE条件。使用含有甲醇和0.1%甲酸溶液的流动相并采用线性梯度洗脱，在C18柱上分离MS-222。通过带有电喷雾离子源的三重四极杆质谱在正模式下进行检测。三种加标水平为0.05、0.5和5μg/L的MS-222回收率在82.6-101%之间，相对标准偏差（RSD）低于9.36%。MS-222的检测限（LOD）和定量限（LOQ）分别为0.01μg/L和0.03μg/L。该方法成功应用于测定从水产品运输车辆或天然集水区采集的实际水样中的MS-222。
