基质分散固相萃取-高效液相色谱-串联质谱法测定鱼肉中吡喹酮和克螨特

HPLC-MS/MS Determination of Praziquantel and Propangite in Fish with Sample Treatment by Matrix Solid Phase Dispersion Extraction

鱼肉样品(2.0g)按基质固相分散萃取法与10mL乙腈以6 000r.min-1转速匀浆1min,随即与4g无水硫酸镁和1.5g氯化钠混合,并以5 000r.min-1转速离心3min,移取上清液1mL,与N-丙基乙二胺和C18粉末各50mg混匀,以10 000r.min-1转速离心3min。取上清液0.5mL与0.5mL水混合,按仪器工作条件进行高效液相色谱-串联质谱法分析。于3种鱼肉样品的基质中分别加入3个浓度水平的混合标准溶液按试验方法做回收试验。测得吡喹酮的回收率在83.7%～93.2%之间,克螨特的回收率在85.2%～92.8%之间,两者测定值的相对标准偏差(n=5)依次在3.7%～9.3%和2.1%～9.6%之间。方法的检出限(3S/N)均为0.3μg.kg-1。

Sample of fish（2.0 g） was treated by MSPD extraction（with 10 mL of CH3CH）,homogenized for 1 min by mixing at a rate of 6 000 r·min-1,and then mixed with 4 g of anhydrous MgSO4 and 1.5 g of NaCl.The mixture was centrifuged for 3 min at a rate of 5 000 r·min-1.One mL of the supernatant was mixed with 50 mg each of N-propyl-ethylene diamine and C18 powder.The mixture was centrifuged for 3 min at a rate of 10 000 r·min-1 and 0.5 mL of supernatant was mixed with 0.5 mL of water and analyzed by HPLC-MS/MS under prescribed conditions.Tests for recovery were made by addition of mixed standard solution at 3 concentration levels to matrixes of 3 kinds of fishes,giving results of recovery in the ranges of 83.7%-93.2% for praziquantel and 85.2%-92.8% for propargite,with values of RSD′s（n=5） ranged from 3.7% to 9.3% and 2.1% to 9.6% respectively.Values of detection limits（3S/N） were found same as 0.3 μg·kg-1.