Determination of Polycyclic Aromatic Hydrocarbons in Chinese Herbal Medicines by Gas Chromatography－Mass Spectrometry with Fe3O4@SiO2@NH2@C60 Magnetic Solid Phase Extraction

SONG Zhong-rong; ZHOU Xiang; JIANG Qing-xiang; YAN Zhi-hong; CAI Ying; LI Hui

doi:10.19969/j.fxcsxb.22101704

您当前的位置：

首页 >

文章列表页 >

Determination of Polycyclic Aromatic Hydrocarbons in Chinese Herbal Medicines by Gas Chromatography－Mass Spectrometry with Fe₃O₄@SiO₂@NH₂@C₆₀ Magnetic Solid Phase Extraction

Scientific Papers | 更新时间：2023-02-28

- Determination of Polycyclic Aromatic Hydrocarbons in Chinese Herbal Medicines by Gas Chromatography－Mass Spectrometry with Fe₃O₄@SiO₂@NH₂@C₆₀ Magnetic Solid Phase Extraction
- Journal of Instrumental Analysis Vol. 42, Issue 2, Pages: 131-140(2023)
- 作者机构：
  
  1.江西中医药大学药学院，江西南昌 330004
  2.中国中医科学院中医药健康产业研究所，江西南昌 330029
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.22101704
  CLC：
扫描看全文
宋中荣,周翔,蒋青香等.基于Fe₃O₄@SiO₂@NH₂@C₆₀的磁固相萃取/气相色谱－质谱联用检测中药材中多环芳烃[J].分析测试学报,2023,42(02):131-140.

SONG Zhong-rong,ZHOU Xiang,JIANG Qing-xiang,et al.Determination of Polycyclic Aromatic Hydrocarbons in Chinese Herbal Medicines by Gas Chromatography－Mass Spectrometry with Fe₃O₄@SiO₂@NH₂@C₆₀ Magnetic Solid Phase Extraction[J].Journal of Instrumental Analysis,2023,42(02):131-140.
宋中荣,周翔,蒋青香等.基于Fe₃O₄@SiO₂@NH₂@C₆₀的磁固相萃取/气相色谱－质谱联用检测中药材中多环芳烃[J].分析测试学报,2023,42(02):131-140. DOI： 10.19969/j.fxcsxb.22101704.

SONG Zhong-rong,ZHOU Xiang,JIANG Qing-xiang,et al.Determination of Polycyclic Aromatic Hydrocarbons in Chinese Herbal Medicines by Gas Chromatography－Mass Spectrometry with Fe₃O₄@SiO₂@NH₂@C₆₀ Magnetic Solid Phase Extraction[J].Journal of Instrumental Analysis,2023,42(02):131-140. DOI： 10.19969/j.fxcsxb.22101704.

摘要

基于Fe,3,O,4,@SiO,2,@NH,2,@C,60,磁纳米复合材料，建立了磁固相萃取/气相色谱－质谱联用同时测定中药材中16种多环芳烃（PAHs）含量的分析方法。采用傅里叶变换红外光谱仪、扫描电镜和振动样品磁力计对复合材料进行表征，证实C,60,改性成功；吸附性能实验结果表明，Fe,3,O,4,@SiO,2,@NH,2,@C,60,的吸附能力强，稳定性好，经10次重复利用后吸附效率无明显变化。考察了萃取溶剂种类、吸附剂用量、吸附时间、解吸溶剂种类以及解吸时间对中药材样品中16种PAHs萃取效率的影响。结果显示，10 mg吸附剂在4 min内即可实现对目标物的完全吸附。采用最优的磁固相萃取条件，16种PAHs在5 ~ 1 000 µg/L范围内具有良好的线性关系，相关系数（,r,2,）为0.994 0 ~ 0.999 9，检出限为0.2 ~ 1.2 µg/kg，定量下限为0.8 ~ 3.9 µg/kg，3个水平下的加标回收率为84.1% ~ 104%，相对标准偏差（RSD）为0.70% ~ 8.3%，日内RSD为0.20% ~ 3.5%，日间RSD为2.2% ~ 6.9%。所建立的方法能有效降低中药材样品中复杂基质的干扰，为中药材中PAHs含量的测定提供了一种操作简便、灵敏度高、准确性好的方法参考。

Abstract

A gas chromatography－mass spectrometry with magnetic solid phase extraction based on Fe,3,O,4,@SiO,2,@NH,2,@C,60, magnetic nanocomposites was established for the simultaneous determination of 16 polycyclic aromatic hydrocarbons（PAHs） in Chinese herbal medicines in this paper．The composites were characterized by Fourier transform infrared spectroscopy，scanning electron microscopy and vibrating sample magnetometer to confirm the successful modification of C,60,．Meanwhile，adsorption experiments were conducted，which showed that the magnetic nanocomposites had a strong adsorption capacity and good stability，and the adsorption efficiency did not change significantly after 10 times of reuse．The effects of extraction solvent type，sorbent dosage，adsorption time，desorption solvent type and desorption time on the extraction efficiency for 16 PAHs in herbal samples were investigated．The results showed that the complete adsorption of 10 mg of sorbent on the targets could be achieved within 4 min．Under the optimal magnetic solid phase extraction conditions，there were good linear relationships for 16 PAHs in the range of 5－1 000 µg/L，with correlation coefficients（,r,2,） of 0.994 0－0.999 9．The limits of detection and the limits of quantitation were in the range of 0.2－1.2 µg/kg and 0.8－3.9 µg/kg，respectively．The spiked recoveries at three levels ranged from 84.1% to 104%，with relative standard deviations（RSDs） of 0.70%－8.3%，intra-day RSDs of 0.20%－3.5% and inter-day RSDs of 2.2%－6.9%．The developed method could effectively reduce the interference on PAHs targets from complex matrices in Chinese herbal medicine samples，and provide an easy-to-operate，sensitive and accurate method reference for the determination of PAHs in Chinese herbal medicines.

关键词

多环芳烃磁纳米粒子C60磁固相萃取/气相色谱－质谱联用中药材

Keywords

polycyclic aromatic hydrocarbonsmagnetic nanospheresC60magnetic solid phase extraction/gas chromatography－mass spectrometryChinese herbal medicines

references

Wu Q N，Shao Y，Gu W，Wang X S．Mod. Chin. Med. （吴启南，邵莹，谷巍，王新胜．中国现代中药），2013，15（3）：169－174.

Bostrom C E，Gerde P，Hanberg A，Jernstrom B，Johansson C，Kyrklund T，Rannug A，Tornqvist M，Victorin K，Westerholm R．Environ. Health Perspect.，2002，110（3）：451－488.

Kim K H，Jahan S A，Kabir E，Brown R J C．Environ. Int.，2013，60：71－80.

Wang B L，Pang S T，Zhang X L，Li X L，Sun Y G，Lu X M，Zhang Q，Zhang Z D．Atmos. Pollut. Res.，2014，5（2）：292－302.

Stallings－Smith S，Mease A，Johnson T M，Arikawa A Y．Environ. Res.，2018，166：588－594.

Wang Y R，Tang Z S，Song Z X，Shi Y J，Xie W．Mod. Chin. Med. （王月茹，唐志书，宋忠兴，史亚军，谢伟．中国现代中药），2017，19（2）：221－225.

Sun X Z，Du J W，Qian Q Q，Wu P G．J. Instrum. Anal. （孙细珍，杜佳炜，钱全全，吴平谷．分析测试学报），2021，40（5）：732－739.

Ishizaki A，Sito K，Kataoka H．Anal. Methods，2018，166：588－594.

Krajian H，Odeh A．Toxicol. Environ. Chem.，2013，95（6）：942－953.

Yu L，Cao Y，Zhang J，Cui Z， Sun H．Food Addit. Contam. Part A，2012，29（11）：1800－1809.

Szternfeld P，Marchi J，Malysheval S V，Joly L．Food Anal. Methods，2019，12（10）：2383－2391.

Yu L F，Cui Z Y，Cao Y Z，Zhang J J，Sun H W．J. Liq. Chromatogr. Relat. Technol.，2015，38（20）：1783－1788.

Cui Z Y，Ge N，Zhang A，Liu Y M，Zhang J J，Cao Y Z．Anal. Bioanal. Chem.，2015，407：1989－1997.

Yu B，Zhang D，Tang L H，Zhao S P，Wang J W，Yao L，Cao W G．RCS Adv.，2017，7（8）：4671－4680.

Garballo－Rubio A，Soto－Chinchilla J，Martín－Pozo L，Zafra－Gómez A．J. Food Compos. Anal.，2020，93：103588.

Shi Z H，Yan J J，Ma Y，Zhang H Y．Procedia Environ. Sci.，2011，10B：1216－1221.

Rozentale I，Lun A Y，Zacs D，Bartkevics V．Food Control，2018，83：45－53.

Asfaram A，Dil E A，Arabkhani P，Sadeghfar F，Ghaedi M．Talanta，2020，218：121131.

He X Q，Cui Y Y，Zhang Y，Yang C X．J. Chromatogr. A，2021，1651：462347.

Peng J B，Ma X G，Chen Y．J. Instrum. Anal. （彭俊标，马晓国，陈圆．分析测试学报），2021，40（6）：960－964.

Kubo T，Murakami Y，Naito T，Otsuka K．Chromatography，2015，36（3）：105－113.

Kubo T，Murakami Y，Tominaga Y，Naito T，Sueyoshi K，Yan M，Otsuka K．J. Chromatogr. A，2014，1323：174－178.

Urbaszek P，Gajewicz A，Sikorska C，Haranczyk M，Puzyn T．Beilstein J. Nanotechnol.，2017，8：752－761.

Lima J D M，Gomes D S，Frazão N F，Soares D J B，Sarmento R G．J. Mol. Model.，2020，26（5）：110.

Nguyen M N，Weidler P G，Schwaiger R，Schafer A I．J. Hazard. Mater.，2021，402：122929.

Yang K，Xing B S．Environ. Pollut.，2007，145：529－537.

Yan Z H，Yuan J B，Zhu G H，Zou Y，Chen C Y，Yang S L，Yao S Z．Anal. Chim. Acta，2013，780：28－35.

Zhou D B，Han F，Ding L，Song W，Lv Y N，Hu Y Y，Liu Y X，Sheng X，Zheng P．J. Chromatogr. B，2020，1144：122076.

Mehdinia A，Khodaee N，Jabbari A．Anal. Chim. Acta，2015，868：1－9.

Liu X F，Lu X，Huang Y，Liu C W，Zhao S L．Talanta，2014，119：341－347.

Zhang S X，Niu H Y，Cai Y Q，Shi Y L．Anal. Chim. Acta，2010，665（2）：167－175.

DB 34/T 3304－2018. ofDetermination 16 Sixteen Polycyclic Aromatic Hydrocarbons in Chinese Medicinal Herbs－GC－MS Method. Anhui Provincial Standard（中草药中16种多环芳烃的测定气相色谱－质谱法．安徽省地方标准）.

Serrano A，Gallego M．J. Sep. Sci.，2006，29（1）：33-40.

Yang X P，Yin Y R，Zong Y Y，Wan T，Liao X J．Microchem. J.，2019，145：26－34.

Qin S B，Fan Y H，Mou X X，Li X S，Qi S H．J. Chromatogr. A，2018，1568：29－37.

Li W B，Chi Y Y，Cheng F．Anal. Test. Technol. Instrum. （李文斌，池艳艳，程菲．分析测试技术与仪器），2022，28（1）：68－79.

Views

下载量

CSCD

Alert me when the article has been cited

提交

Tools

Publicity Resources

Determination of Polycyclic Aromatic Hydrocarbons in Environmental Water by HPLC with Stir Bar Adsorption Extraction Based on Covalent Organic Framework Coating

Determination of PAHs and OPFRs in Atmospheric Particulate Matters by High Performance Solvent Extraction－Solid Phase Extraction/Gas Chromatography－Mass Spectrometry

Rapid Screening of Polycyclic Aromatic Hydrocarbons in Food Contact Materials by Surface-enhanced Raman Spectroscopy Combined with Principal Component Analysis

Simultaneous Determination of 65 Polychlorinated Biphenyls,Polycyclic Aromatic Hydrocarbons and Organochlorine Pesticides in Marine Sediments by GC-MS with Accelerated Solvent Extraction

Related Author

No data

Related Institution

Provincial Key Laboratory of Gansu Higher Education for City Environmental Pollution Control

School of Chemistry and Chemical Engineering，Lanzhou City University

Provincical Key Laboratory of Gansu Higher Education for City Environmental Pollution Control

Environment Research Institute，Shandong University

Jinan Eco-environmental Monitoring Center of Shandong Province

Address：100 Xianlie Middle Road, Guangzhou Postal code：510070
Tel：020-87684776,37656606 Fax：020-87684776 Email：fxcsxb@china.com
Technical support is provided by Beijing Founder electronics co., LTD 粤ICP备12017312号-3 京公网安备11010802024621
It is recommended to read the content of this site in Chrome&IE9+. Please switch to extreme mode in browser 360.
Cookies We use cookies to help provide and enhance our service and tailor content. By continuing, you agree to the use of cookies.

⁰