超高效液相色谱-质谱联用法测定消毒产品中30种糖皮质激素

Determination of 30 species of glucocorticoid in disinfection products by UPLC-MS / MS

目的建立消毒产品中30种糖皮质激素的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。方法以饱和氯化钠溶液及乙腈2次液液萃取样品后做沉淀蛋白处理,提取液经过固相萃取小柱净化浓度后采用C18色谱柱分离(100 mm×2.1 mm,1.7μm)。以乙腈和水(含0.1%甲酸)为色谱分离流动相进行梯度洗脱,多反应监测模式进行定性分析和定量分析。结果 30种糖皮质激素以标准曲线-外标法定量,其在0 ng/ml^50.0 ng/ml时,线性关系良好,相关系数(r)≥0.995;定量限(S/N=10)为0.002 ng/ml^0.6 ng/ml。分别加入浓度为5.0 ng/ml和25.0 ng/ml的标准溶液,其回收率为58.7%~146.8%,相对标准偏差(RSD)为1.22%~19.21%。结论本法操作简便、灵敏度高,适用于消毒产品中糖皮质激素的检测。

Objective To establish a method for the determination of 30 species of glucocorticoid in disinfection products by ul- tra performance liquid chromatography tandem mass spectrometry（ UPLC - MS/MS）. Methods Before precipitation of protein, the samle was disovled by saturated sodium chloride solution and extracted by acetonitfile twice, the extracted solution was con- centrated and purified with solid phase extraction column （SPE）. The eluate were separated by a ClS column （ 100 mm× 2.1 mm, 1.7 μm）. With acetonitrile and water（0.1% formic acid） as the chromatographic separation mobile phase for gradi- ent elution, multi reaction monitoring mode was used for qualitative analysis and quantitative analysis. Results 30 kinds of glucocorticoids were quantified with standard curve and standard quantitative method and good linearity was obtained when the concentration of it was within 0 ng/ml - 50.0 ng/ml, with correlation coefficient（r） equal to or greater than 0. 995 ; the limit of quantification （ S/N = 10） was within 0. 002 ng/ml - 0.6 ng/ml ; adding the standard solution with the concentration of 5.0 ng/ml and 25.0 ng/rnl. The recovery rate was within 58.7% - 146.8% , and the relative standard deviation（RSD） was within 1.22% - 19.21%. Conclusion The method is simple, sensitive and accurate. It is suitable for the determination of glucocorticoid in disinfectants.