QuEChERS净化-超高效液相色谱串联质谱法测定“消”字号抑菌产品中50种糖皮质激素

Determination of fifty kinds of glucocorticoids in antibacterial products with"Xiao"brand by QuEChERS purification coupled with ultra high performance liquid chromatography-tandem mass spectrometry

建立了超高效液相色谱-串联质谱法检测“消”字号抗抑菌产品中50种糖皮质激素的分析方法。样品采用饱和氯化钠溶液分散,乙腈溶液振荡及超声提取,QuEChERS分散固相萃取剂净化,Agilent Eclipse Plus C_(18)RRHD色谱柱(100 mm×2.1 mm,1.8μm)分离,甲醇-0.1%乙酸溶液梯度洗脱,多反应监测正离子模式检测,外标法定量。结果表明,在优化的色谱条件下,11对糖皮质激素同分异构体分离良好。50种糖皮质激素在0~100μg/L浓度范围内线性关系良好,相关系数(r)均大于0.995。在样品基质中添加浓度水平为0.3,0.8,1.6 mg/kg的标准溶液,方法的平均回收率为76.9%~106.6%,相对标准偏差(RSD)在2.2%~9.9%之间,方法定量限在0.03~0.10 mg/kg之间。对30批次“消”字号抗抑菌产品进行糖皮质激素筛查,有4批次检出糖皮质激素。该方法可用于“消”字号抗抑菌产品中糖皮质激筛查定量。

A method for the determination of 50 glucocorticoids in"Xiao"anti-bacteriostatic products by ultra-high performance liquid chromatography-tandem mass spectrometry was established.The sample was dispersed in saturated sodium chloride solution,thereafter oscillated by acetonitrile solution and extracted by ultrasound,followed by purification via QuEChERS dispersed solid phase extractant,and separated by Agilent Eclipse Plus C_(18)RRHD column(100 mm×2.1 mm,1.8μm).The gradient elution was performed by methanol-0.1%acetic acid solution,and the target was detected by multi-reaction monitoring positive ion mode,and quantified by external standard method.The results showed that 11 pairs of glucocorticoid isomers were well separated under optimal chromatographic conditions.The linear relationships of 50 glucocorticoids were satisfactory in the concentration range of 0-100μg/L,and the correlation coefficients(r)were all greater than 0.995.When 0.3,0.8 and 1.6 mg/kg standard solutions were added to the sample matrix,the average recoveries were obtained in the range of 76.9%-106.6%,the relative standard deviations(RSDs)were 2.2%-9.9%,and the limits of quantitation of the method were 0.03-0.10 mg/kg.Glucocorticoids were found in four batches from thirty batches of the antibacterial products.The method is capable of utilizing for screening and quantifying glucocorticoids in antibacterial products,providing a technical support for supervision of antibacterial products with"Xiao"brand.