Study on the simultaneous measurement of residual level of three pesticides in nelumbinis semen using GC-MS/MS / 国际中医中药杂志

Objective To establish a quantitative method for the simultaneous measurement of the residual level of three pesticides in Nelumbinis semen by GC-MS/MS. Methods The samples were extracted by acetonitrile and purify by Cleanert TPH column. The samples were then tested by GC-MS/MS. Information on relative retention time and mass charge ratio was used for qualitative analysis. The peak area obtained by secondary ion MS of bifenthrin (181.1/166.1)was used as the reference peak to calculate the relative correction factor for the peak area of fenpropathrin (265.1/210.1) and deltamethrin (252.9/93.0), to establish a method using bifenthrin as the reference substance to determinate there sidual quantity of three pesticides in Nelumbinis semen by GC-MS/MS. Results When the injection quantity of the sample containing bifenthrin,fenpropathrin and deltamethrin in the range of 0.01-0.1 ng , there was a good linear relationship between the injection quantity and peak are a Limitation of quantification (LOQ) of bifenthrin , fenpropathrin and deltamethrin were 4.321×10-4 ng, 3.435×10-4 ng, 8.913×10-3 ng, respectively. The average recovery rates of bifenthrin, fenpropathrin and deltamethrin were 93.5％, 93.5％ and 93.8％, respectively. Conclusions The method of quantitative analysis of multi-components with a single-marker is simple, quick and accurate. It suitable for the detection of residual quantity of bifenthrin, fenpropathrin and deltamethrin in Nelumbinis semen.

Determination of Sulfurous Anhydride in Rhizoma Dioscoreae by Ion Chromatography-Direct Extraction / 中国药师

Objective:To establish a quantitative analysis method to determine the content of sulfurous anhydride in Rhizoma di-oscoreae by ion chromatography-direct extraction. Methods:Sulfurous anhydride was extracted by KOH solution (25 mmol·L-1). An IonPac? AS11-HC column(250 mm × 4 mm, 9. 0 μm) was used. The column temperature was 20℃, the eluent was KOH solution (20 mmol·L-1 ) at flow rate of 1. 00 ml·min-1 and the conductivity temperature was 20℃. Results:There was a good linear rela-tionship between the injection quantity (1.160-29.100 μg)and the peak area of sulfite(r =0.999 9). The average recovery was 98. 9%(RSD=0. 6%, n=9). The quantitation limit was 1. 38 ng·ml-1. Conclusion: The method is simple, accurate and rapid, which is appropriate for the quantitative analysis of sulfite anhydride in Rhizoma dioscoreae.