【摘要】：建立了分散固相萃取-液相色譜-串聯(lián)質(zhì)譜同時快速測定化妝品中81種非法添加糖皮質(zhì)激素(GCs)的分析方法。樣品用水分散后加乙腈超聲提取,經(jīng)十八烷基鍵合硅膠(C18)和N-丙基乙二胺(PSA)凈化,待測物選用具有多重色譜保留模式的Poroshell 120 PFP色譜柱(100 mm×2.1 mm,2.7μm)分離,以0.2%(v/v)乙酸水溶液-乙腈為流動相梯度洗脫,在電噴霧正離子模式下以動態(tài)多反應(yīng)監(jiān)測方式測定,內(nèi)標(biāo)法定量。81種待測物在各自的濃度范圍內(nèi)線性關(guān)系良好,相關(guān)系數(shù)均大于0.99,在3個不同的添加水平下,平均回收率為68.8%~105.3%,RSD為2.9%~13.1%(n=6),方法的檢出限(S/N≥3)和定量限(S/N≥10)分別為0.002~0.006μg/g和0.005~0.020μg/g。篩查了137個化妝品樣品,發(fā)現(xiàn)16個陽性樣品,含量為16.9~158μg/g。結(jié)果表明,該法簡便快速,靈敏可靠,適用于化妝品中81種GCs的同時快速定性定量篩查分析。
[Abstract]:A rapid method for the simultaneous determination of 81 illegal corticosteroids (GCs) in cosmetics by dispersion solid-phase extraction liquid chromatography-tandem mass spectrometry was established. The samples were separated by water dispersion and ultrasonic extraction with acetonitrile. The samples were purified by octadecyl bonded silica gel (C18) and N-propyl ethylenediamine (PSA). The samples were separated on a Poroshell 120 PFP column (100 mm 脳 2.1 mm, 2.7 渭 m) with multiple chromatographic retention mode. Using 0.2% (vv) acetic acid aqueous solution-acetonitrile as mobile phase gradient elution, dynamic multi-reaction monitoring method was used in electrospray positive ion mode, and the internal standard method was used for quantitative analysis. 81 kinds of compounds were linear in their respective concentration range. The correlation coefficients were all more than 0.990.The average recovery was 68.8% and 105.3%, RSD was 2.9% and 13.1% (n = 6) at three different levels of addition, and the average recovery was 68.8% and 105.3% (RSD = 2.9% and 13.1%, n = 6), respectively. The detection limits and quantitative limits of the method were 0.002 ~ 0.006ug / g and 0.0050.020ug / g, respectively. The detection limit and quantitative limit were 0.0020.006ug / g and 0.0050.020ug / g, respectively. 137 cosmetics samples were screened and 16 positive samples were found, the content was 16.9 ~ 158 渭 g / g. The results showed that the method was simple, rapid, sensitive and reliable. It was suitable for the simultaneous qualitative and quantitative analysis of 81 kinds of GCs in cosmetics.
【作者單位】： 中國廣州分析測試中心廣東省化學(xué)危害應(yīng)急檢測技術(shù)重點實驗室;
【基金】：廣東省省級科技計劃項目(2014A040401038,2014B070705001)~~
【分類號】：O657.63;TQ658

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