65%氨氟乐灵水分散粒剂的高效液相色谱-质谱和气相色谱-质谱分析方法

Analytical method for prodiamine 65% WG by HPLC-MS and GC-MS

建立了利用高效液相色谱串联质谱(HPLC-MS)和气相色谱串联质谱(GC-MS)测定氨氟乐灵水分散粒剂中有效成分含量的方法。HPLC-MS法采用Zorbax Eclipse XDB-C18色谱柱,以甲醇-0.2%乙酸水(体积比80∶20)为流动相,通过ESI离子源负离子模式扫描测定氨氟乐灵含量。GC-MS法以HP-5MS毛细管柱为分离柱,以氦气为载气,通过EI离子源SIM模式测定氨氟乐灵的含量。结果表明,HPLC-MS和GC-MS分析方法的线性相关性分别为1.000 0和0.999 6,标准偏差分别为0.23和0.32,变异系数分别为0.36%和0.49%,回收率分别为98.12%~101.35%和99.77%~101.91%。两种方法均操作简便,准确度和精密度较高,可准确分析氨氟乐灵水分散粒剂中有效成分含量。

Two methods were developed for the determination of prodiamine water dispersible granule using HPLC-MS and GC-MS.The HPLC-MS method was performed on a Zorbax Eclipse XDB-C18 column with methanol and 0.2% acetic acid water(80∶20,v∶v) as the mobile phase,and the content of prodiamine was determined by scanning in negative ion mode with an ESI ion source.The GC-MS method was used to determine the content of amiloride by EI ion source SIM mode with a HP-5MS capillary column as the separation column and helium gas as the carrier gas.Result showed that the linear correlation coefficients of HPLC-MS and GC-MS methods were 1.000 0 and 0.999 9,the standard deviations were 0.23 and 0.32,the variation coefficients were 0.36% and 0.49%,and the recoveries were 98.12%~101.35% and 99.77%~101.91%,respectively.Both methods are easy to operate with high accuracy and precision,and can accurately determine the content of the active ingredients in prodiamine water dispersible granule.