Establishment of modified gas chromatography-mass spectrometry for determination of plasma sufentanil concentrations / 中华麻醉学杂志

ABSTRACT

Objective To modify gas chromatography-mass spectrometry (GC-MS) for determination of plasma sufentanil concentrations.Methods Fentanyl was used as the internal standard.The plasma samples were extracted with ethyl acetate and petroleum ether.An HP-5MS capillary column was used.The initial temperature of the column was set at 130 ℃,and the final temperature was 320 ℃.The injector port temperature was set at 290 ℃,and the interface temperature was 300 ℃.The carrier gas was high purity helium (purity 99.999％) with a constant flow rate of 1 ml/min.The injection volume was 1 μl with splitless injection.The MS conditions were as followsEI source,ion source temperature 230 ℃,four-pole temperature 150 ℃,electron bombardment energy 70 eV,multiply voltage 2112 V,selective ion monitoring mode,solvent delay 7 min.The characteristic ions of sufentanil and fentanyl were obtained in 8.20-8.40 min and 7.60-7.80 min,respectively,according to the characteristic ion curve of sufentanil and fentanyl.Results The standard curve of sufentanil had good linear relationship in the range of 0.02-10.00 ng/ml and the equation was Y =0.1625X + 0.0316,R2 =0.9987.The extraction recovery was more than 80％,intra-day and inter-day determinations were less than 8％,and the limit of detection was 0.02 ng/ml.Conclusion When modified GC-MS is applied to determine the concentrations of sufentanil in plasma,not only the determination is sensitive and accurate,but also the procedures are simplified,and it is more suitable for the pharmacological research of sufentanil.