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[采用快速去除磷脂固相萃取法-超高效液相色谱串联质谱法测定人体血液中的双酚A]

[Determination of bisphenol A in human blood by using fast phospholipid removal solid phase extraction method-ultra performance liquid chromatography tandem mass spectrometry].

作者信息

Qin Yanyan, Jian Bin, Guo Gang, Niu Yingfang

机构信息

Shenzhen Polytechnic, Shenzhen 518055, China.

出版信息

Wei Sheng Yan Jiu. 2018 Jan;47(1):134-140.

Abstract

OBJECTIVE

To develop a method for determination of bisphenol A in human blood by fast phospholipid removal solid phase extraction method-ultra performance liquid chromatography tandem mass spectrometry( UPLC-MS/MS).

METHODS

Enzymatic hydrolysis( β-glucuronidase/arylsulfatase) and phospholipid removal solid phase extraction were used to treat the blood samples under the acidic condition, a Infinity Lab Poroshell 120 PFP column( 100 mm × 3. 0 mm, 2. 7 μm) was used for LC separation, ESI negative ion scan was used with multiple reaction monitoring( MRM) mode.

RESULTS

The calibration curve was linear in the range of 0. 1-100 ng/mL for bisphenol A with correlation coefficients more than 0. 999. The limit of detection was 0. 05 ng/mL, the limit of quantity was 0. 15 ng/mL. The recoveries of the method for bisphenol A at three spiked levels of 0. 5, 5 and 50 ng/mL ranged from 87. 3%to 112. 1%. The relative standard deviation( RSD) of intra and inter day were range from3. 3%-8. 2%, 4. 9%-10. 7%( n = 6), respectively.

CONCLUSION

The method is successfully applied in the analysis of bisphenol A in human blood with its simple operation, sensitivity and accuracy.

摘要

目的

建立一种快速去除磷脂固相萃取-超高效液相色谱串联质谱法(UPLC-MS/MS)测定人血液中双酚A的方法。

方法

采用酶水解(β-葡萄糖醛酸苷酶/芳基硫酸酯酶)和酸性条件下去除磷脂固相萃取法处理血样,以Infinity Lab Poroshell 120 PFP柱(100 mm×3.0 mm,2.7μm)进行液相色谱分离,采用电喷雾负离子扫描和多反应监测(MRM)模式。

结果

双酚A校准曲线在0.1~100 ng/mL范围内呈线性,相关系数大于0.999。检出限为0.05 ng/mL,定量限为0.15 ng/mL。双酚A在0.5、5和50 ng/mL 3个加标水平下的回收率为87.3%~112.1%。日内和日间相对标准偏差(RSD)分别为3.3%~8.2%、4.9%~10.7%(n = 6)。

结论

该方法操作简便、灵敏、准确,成功应用于人血液中双酚A的分析。

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