【摘要】：建立了QuEChERS-同位素稀釋-液相色譜-四極桿串聯(lián)飛行時(shí)間質(zhì)譜同時(shí)快速篩查化妝品中86種糖皮質(zhì)激素(Glucocorticoids,GCs)的高通量方法。樣品經(jīng)乙腈提取,改進(jìn)的QuEChERS法凈化,待測物選用具有多重色譜保留機(jī)理的新型色譜柱Poroshell 120 PFP(100 mm×2.1 mm,2.7μm),以0.2%(V/V)乙酸和乙腈為流動(dòng)相進(jìn)行梯度洗脫分離,在電噴霧離子源的正離子模式下建立了一級(jí)精確質(zhì)量數(shù)及二級(jí)碎片離子質(zhì)譜圖數(shù)據(jù)庫,無需標(biāo)準(zhǔn)品即可完成化妝品中86種GCs的全面篩查與確證。所有待測物在2~200μg/L濃度范圍內(nèi)線性良好,相關(guān)系數(shù)均大于0.99,3個(gè)添加水平的平均回收率為66.2%~112.8%,相對(duì)標(biāo)準(zhǔn)偏差(RSD)為4.6%~13.9%,檢出限(LOD,S/N≥3)為0.006~0.015 mg/kg,定量限(LOQ,S/N≥10)為0.02~0.05 mg/kg。本方法簡便高效、定性可靠、定量準(zhǔn)確,適用于化妝品中非法添加GCs的高通量篩查。
[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，

本文編號(hào)：2216098