QuEChERS-同位素稀释-液相色谱-高分辨飞行时间质谱法高通量筛查化妆品中86种糖皮质激素
发布时间：2018-08-31 20:40
【摘要】：建立了QuEChERS-同位素稀释-液相色谱-四极杆串联飞行时间质谱同时快速筛查化妆品中86种糖皮质激素(Glucocorticoids,GCs)的高通量方法。样品经乙腈提取,改进的QuEChERS法净化,待测物选用具有多重色谱保留机理的新型色谱柱Poroshell 120 PFP(100 mm×2.1 mm,2.7μm),以0.2%(V/V)乙酸和乙腈为流动相进行梯度洗脱分离,在电喷雾离子源的正离子模式下建立了一级精确质量数及二级碎片离子质谱图数据库,无需标准品即可完成化妆品中86种GCs的全面筛查与确证。所有待测物在2~200μg/L浓度范围内线性良好,相关系数均大于0.99,3个添加水平的平均回收率为66.2%~112.8%,相对标准偏差(RSD)为4.6%~13.9%,检出限(LOD,S/N≥3)为0.006~0.015 mg/kg,定量限(LOQ,S/N≥10)为0.02~0.05 mg/kg。本方法简便高效、定性可靠、定量准确,适用于化妆品中非法添加GCs的高通量筛查。
[Abstract]:A high throughput method for rapid screening of 86 glucocorticoids (Glucocorticoids,GCs) in cosmetics by QuEChERS- isotope dilution liquid chromatography-quadrupole tandem time-of-flight mass spectrometry was established. The samples were extracted by acetonitrile and purified by improved QuEChERS method. A new column, Poroshell 120 PFP (100 mm 脳 2.1 mm,2.7 渭 m),) with retention mechanism of multiplex chromatography, was used for gradient elution and separation with 0.2% (V / V) acetic acid and acetonitrile as mobile phase. Under the positive ion mode of the electrospray ion source, the first order accurate mass number and the second order fragment ion mass spectrogram database were established. The comprehensive screening and confirmation of 86 kinds of GCs in cosmetics could be completed without the standard. All the samples were linear in the concentration range of 2 ~ 200 渭 g / L, the correlation coefficient was greater than 0.99, the average recovery of the three additive levels was 66.2 ~ 112.8, the relative standard deviation (RSD) was 4.6g / L, the detection limit (LOD,S/N 鈮，
本文编号：2216098
[Abstract]:A high throughput method for rapid screening of 86 glucocorticoids (Glucocorticoids,GCs) in cosmetics by QuEChERS- isotope dilution liquid chromatography-quadrupole tandem time-of-flight mass spectrometry was established. The samples were extracted by acetonitrile and purified by improved QuEChERS method. A new column, Poroshell 120 PFP (100 mm 脳 2.1 mm,2.7 渭 m),) with retention mechanism of multiplex chromatography, was used for gradient elution and separation with 0.2% (V / V) acetic acid and acetonitrile as mobile phase. Under the positive ion mode of the electrospray ion source, the first order accurate mass number and the second order fragment ion mass spectrogram database were established. The comprehensive screening and confirmation of 86 kinds of GCs in cosmetics could be completed without the standard. All the samples were linear in the concentration range of 2 ~ 200 渭 g / L, the correlation coefficient was greater than 0.99, the average recovery of the three additive levels was 66.2 ~ 112.8, the relative standard deviation (RSD) was 4.6g / L, the detection limit (LOD,S/N 鈮，
本文编号：2216098
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