气相色谱及气相色谱—质谱联用技术分析牙菌斑脂肪酸方法的建立

Establishment of a GC and GC/MS Method for Analysis of Fatty Acids in Human Dental Plaque

目的 :建立一种测定牙菌斑脂肪酸的气相色谱、气相色谱 -质谱分析法。方法 :气相色谱检测为柱长 2 5m ,内径 2 5mm ,固定相OV 1;气相色谱 -质谱检测为柱长 2 3m ,内径 0 2 3mm ,固定相OV 1键合相熔融石英毛细管柱 ,检测人牙菌斑中的脂肪酸。结果 :线性回归方程为Y =0 0 138X - 0 1182 ,r =0 9945 ,回收率为 90 18%～10 3 6 % ,CV日内 分别为 2 6 0、1 6 1、2 2 0 ;CV日间 分别为 2 71、1 6 9、1 6 1,最低检测量为 0 6 μg。 结论 :该方法的精密度、可靠性、重复性均较好 ,可用于牙菌斑脂肪酸的检测。

Objective:To study the composition of fatty acids in human dental plaque, a Gas Chromatography (GC) and Gas Chromatography/Mass Spectrometry (GC/MS) method was developed. Methods:The C17:0 was internal standard and the C16:0 was test standard. Samples of plaque were methanolysis to be fatty acids methyl ester before detection. GC with OV_1 separated the sample for a quantitative analysis. The column size was 25m×25mm. The temperature program was from 80℃ to 260℃with 12℃/min. The sample separation was carried out at fused silica capillary column with OV_1 for qualitative analysis by GC/MS. The column size was 23m× 0.23mm. The temperature program was from 40℃ to 240℃ at 6℃/min.Results:The linear regression equation was y=0.0138X-0.1182, r=0.9945, recovery was 90.18%～103.6%, CV intro_day was 2.60、1.61、2.20; CV inter-day was; 2.71、1.69、1.61. The lowest limit of detection was 0.6ug. The GC and GC/MS diagram showed that internal standard and fatty acids of plaque have good separation. Conclusion:The method is simple, rapid accurate, and is useful to carry out qualitative and quantitative analyses of fatty acids in dental plaque.\;