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目的建立解吸附电晕束电离质谱(DCBI-MS)快速检测微量雌激素的分析方法。方法通过DCBI-MS直接分析,对比标准物质一级和二级质谱图,对检测样品中非法添加的炔诺酮、黄体酮、甲羟孕酮、左炔诺孕酮、醋酸甲地孕酮和枸橼酸氯米芬等6种雌激素进行快速定性和半定量检测。结果各目标化合物均可在1 min内被检出。基于一级分子离子的定量分析,6种雌激素的半定量检测结果可信,线性关系最差的醋酸甲地孕酮相关系数为0.9471,而黄体酮则为0.9998。最低检出值分别是0.0875、0.045、0.1775、0.05、0.15、0.1 mg/L。结论本方法无需复杂的前处理过程,简便、快速、灵敏度高,可用于保健食品和中成药中违禁添加微量雌激素的快速定性及半定量检测。
Objective To establish a method for the rapid determination of trace estrogen by desorption corona beam ionization mass spectrometry (DCBI-MS). Methods By DCBI-MS direct analysis, comparing the first and second standard spectra of reference materials, the test samples illegally added norethindrone, progesterone, medroxyprogesterone, levonorgestrel, megestrol acetate and megestrol Clomiphene citrate and other 6 kinds of estrogen rapid qualitative and semi-quantitative detection. Results Each target compound was detected within 1 min. Based on the quantitative analysis of the first-class molecular ions, the semi-quantitative detection results of the six estrogens were credible. The correlation coefficient of megestrol acetate with the worst linear relationship was 0.9471, while that of progesterone was 0.9998. The lowest detection value is 0.0875,0.045,0.1775,0.05,0.15,0.1 mg / L. Conclusion This method does not require complicated pretreatment process. It is simple, rapid and sensitive. It can be used for rapid qualitative and semi-quantitative detection of banned trace estrogen in health food and proprietary Chinese medicines.