气相色谱串联质谱法同时测定鱼金注射液中芳樟醇和甲基正壬酮含量  

Simultaneous Determination of Linalool and Methyl-Nnonylketone in Yujin Injection by GC-MS/MS

作　　者：陈骁勇 葛玉松 CHEN Xiaoyong;GE Yusong(Yancheng No.1 People's Hospital,Yancheng,Jiangsu,China 224000;Yancheng Food and Drug Supervision and Inspection Center,Yancheng,Jiangsu,China 224000)

机构地区：[1]江苏省盐城市第一人民医院,江苏盐城224000 [2]江苏省盐城市食品药品监督检验中心,江苏盐城224000

出　　处：《中国药业》2022年第8期83-85,共3页China Pharmaceuticals

摘　　要：目的建立同时测定鱼金注射液中芳樟醇、甲基正壬酮含量的气相色谱串联质谱(GC-MS/MS)法。方法色谱柱为Agilent19091S-431 HP-5MS毛细管柱(30 m×0.25 mm,0.25μm),程序升温,进样口温度为250℃,流速为1.0 mL/min,顶空进样,加热温度为90℃,平衡45 min,分流比为10∶1;电子轰击离子源,电子能量为70 eV,离子源温度为230℃,MSD传输线温度为280℃,四极杆温度为150℃,淬灭气(氦气)流速为2.25 mL/min,碰撞气(氮气)流速为1.50 mL/min,多反应监测扫描模式。结果芳樟醇、甲基正壬酮质量浓度分别在0.01358~0.13580 mg/mL(r=0.9991,n=6)和0.00609~0.06088 mg/mL(r=0.9987,n=6)范围内与峰面积线性关系良好;精密度、稳定性、重复性试验结果的RSD均小于2.0%;平均加样回收率分别为98.96%和99.82%,RSD分别为1.53%和1.04%(n=6)。结论所建立的方法简便可靠,灵敏度高,重复性好,适用于同时测定鱼金注射液中芳樟醇和甲基正壬酮的含量。Objective To establish a gas chromatography-tandem mass spectrometry(GC-MS/MS)method for the simultaneous determination of linalool and methyl-nonylketone in Yujin Injection.Methods The chromatographic column was Agilent 19091S-431 HP-5MS capillary column(30 m×0.25 mm,0.25μm)with temperature programmed by headspace injection,the injection port temperature was 250℃,the flow rate was 1.0 mL/min,the heating temperature was 90℃and 45 minutes for balance,the split ratio was 10∶1.Electron impact ion source,the electron energy was 70 eV,the ion source temperature was 230℃,the temperature of MSD transmission line was 280℃,the quadrupole temperature was 150℃,the flow rate of quenching gas(helium)was 2.25 mL/min,the flow rate of collision gas(nitrogen)was 1.50 mL/min with the multi reaction monitoring(MRM)mode.Results The mass concentration of linalool and methyl-nnonylketone showed a good relationship with the peak area in the ranges of 0.01358-0.13580 mg/mL(r=0.9991,n=6)and 0.00609-0.06088 mg/mL(r=0.9987,n=6).The RSDs of precision,stability and repeatability tests were less than 2.0%,the average recoveries were 98.96% and 99.82% with RSDs of 1.53%和1.04%(n=6).Conclusion The established method is simple,reliable,sensitive and reproducible,which can be used for the simultaneous determination of linalool and methyl-nnonylketone in Yujin Injection.

关 键 词：气相色谱串联质谱法 鱼金注射液 芳樟醇 甲基正壬酮 同时测定 

分 类 号：R917[医药卫生—药物分析学] R284.1[医药卫生—药学]