全自动固相萃取-超高效液相色谱-串联质谱法测定婴幼儿湿疹类产品中42种糖皮质激素

doi:10.3724/SP.J.1123.2017.10035

色谱 ›› 2018, Vol. 36 ›› Issue (4): 356-361.DOI: 10.3724/SP.J.1123.2017.10035

全自动固相萃取-超高效液相色谱-串联质谱法测定婴幼儿湿疹类产品中42种糖皮质激素

潘小红, 殷帅, 刘玉玲, 龙凌云, 赵薇, 孟庆玉

湖南省食品药品检验研究院, 湖南长沙 410001

收稿日期:2017-11-02 出版日期:2018-04-08 发布日期:2014-02-26
通讯作者: 孟庆玉,Tel:(0731)82275868,E-mail:2496125098@qq.com
基金资助:
湖南省自然科学基金（2016JJ6079）.

Determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry

PAN Xiaohong, YIN Shuai, LIU Yuling, LONG Lingyun, ZHAO Wei, MENG Qingyu

Hunan Institute for Food and Drug Control, Changsha 410001, China

Received:2017-11-02 Online:2018-04-08 Published:2014-02-26
Supported by:
Natural Science Foundation of Hunan Province (No. 2016JJ6079).

摘要/Abstract

摘要：

建立了全自动固相萃取-超高效液相色谱-串联质谱检测婴幼儿湿疹类产品中42种糖皮质激素的方法。样品用饱和氯化钠溶液分散后加乙腈涡旋提取，经亚铁氰化钾和醋酸锌沉淀大分子基质，然后用HLB固相萃取柱净化，待测液用Dikma Endeavorsil^TM C18色谱柱（100 mm×2.1 mm，1.7 μm）分离，以0.1%（v/v）甲酸水溶液-乙腈为流动相进行梯度洗脱。在电喷雾正离子模式下以动态多反应监测方式测定，外标法定量。42种待测物在各自的范围内呈良好的线性关系，相关系数均大于0.998；在3个添加水平下，42种待测物的平均回收率为78.7%~101.5%，RSD为2.0%~8.8%（n=6）；方法的检出限（LOD，S/N≥3）和定量限（LOQ，S/N≥10）分别为0.002~0.031 mg/kg和0.0007~0.103 mg/kg。该法简便快速，灵敏可靠，适用于婴幼儿湿疹类产品糖皮质激素的检测。

关键词: 超高效液相色谱-串联质谱, 糖皮质激素, 婴幼儿湿疹产品, 自动固相萃取

Abstract: A method was developed for the determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-high performance liquid chromatography-tandem mass spectrometry (ASPE-UHPLC-MS/MS).The analytes were extracted by acetonitrile after dispersing in saturated sodium chloride solution.Macromolecules matrix were precipitated by adding potassium and zinc acetate, and then purified by HLB SPE column.The chromatographic separations were performed on a DIKMA EndeavorsilTM C18 column (100 mm×2.1 mm, 1.7 μm).Acetonitrile and 0.1%(v/v) formic acid aqueous solution were used as the mobile phases.Electrospray ionization (ESI) source was operated in the positive mode using multiple reaction monitoring (MRM) scanning mode.The results were quantified by external standard method.The correlation coefficients of linear calibration curves were greater than 0.998 in the corresponding mass concentration ranges.The average recoveries at three spiked levels ranged from 78.7% to 101.5%, and the relative standard deviations (RSDs) were 2.0%-8.8%(n=6).The LODs (S/N ≥ 3) and LOQs were 0.002-0.031 mg/kg and 0.0007-0.103 mg/kg, respectively.The method is simple, rapid, sensitive, and reliable, and can be used for the detection of glucocorticoids in infant eczema products.

Key words: auto-solid phase extraction (ASPE), glucocorticoid, infant eczema products, ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS-MS)

中图分类号:

O658

潘小红, 殷帅, 刘玉玲, 龙凌云, 赵薇, 孟庆玉. 全自动固相萃取-超高效液相色谱-串联质谱法测定婴幼儿湿疹类产品中42种糖皮质激素[J]. 色谱, 2018, 36(4): 356-361.

PAN Xiaohong, YIN Shuai, LIU Yuling, LONG Lingyun, ZHAO Wei, MENG Qingyu. Determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Chinese Journal of Chromatography, 2018, 36(4): 356-361.

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全自动固相萃取-超高效液相色谱-串联质谱法测定婴幼儿湿疹类产品中42种糖皮质激素

Determination of 42 glucocorticoids in infant eczema products by auto-solid phase extraction-ultra high performance liquid chromatography-tandem mass spectrometry

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