FAB-MS总离子流非线性拟合法分析川芎嗪___

Abstract Objective: Our laboratory have found a new method for the measurement of ligustrazine using fast atom bombardment mass spectrometry (FAB–MS). Method: It was found that the total ion’s intensity of quasi-ion molecule took on exponential decrease. Fitting it by non –liner curve could calculate the initiatory total ion’s intensity. The quasi-ion molecule peak initiatory total intensity ratio of the sample and internal standard was proportion to the concentration of tested sample; it could be applied to quantitative analysis. In this work ligustrazine was determined quantitatively by using above conclusion and internal standard was deuteride itself. The preparation of internal standard was carried out with two deuterated reagent, heavy water and deuterated methanol respectively with two radiation irradiation, laser and ultraviolet. The deuterated rate was determined by EI-MS, according to the difference of I₁₃₆/I₁₃₇ of deuterated and undeuterated ligustrazine. Deuterated methanol as deuterated reagent was better, and it’s deuteration rate was 2.43% under laser radiation for 0.5 h. Ligustrazine was analyses by FAB-MS with glycol as matrix in the presence of deuterated, ligustrazine as internal standard. The mass spectrometer conditions were as follow: the ionization mode was FAB, resolution, 1000, gun voltage 8kV, and gun gas, Ar. Result: A standard equation for analyses ligustrazine was set up, which was Y = 6.75+2.24 X  (r= 0.9908), RSD was 2.9 %. In this paper troche medicine of ligustrazine phosphate has been quantitative analysis, in which the results of two different pre-treatments were compared.and results were 43.0 mg per piece and 45.0 per piece. Conclusion: This method is available to analyze quantitatively the sample of ligustrazine with little interference, high precision and microgramme samples.