目的 建立GC-MS/MS测定中药材中16种多环芳烃的残留量,为评价中药质量安全提供有效分析手段。方法 采用同位素内标法,样品以乙酸乙酯提取后,经C18固相萃取小柱净化。GC-MS/MS测定,加入分析保护剂校正基质效应,色谱柱为DB-5 ms(0.25 mm×30 m,0.25 μm),程序升温,MRM模式检测。结果 16种典型多环芳烃在1~100 ng·mL-1内呈线性关系;在1~25 μg·kg-1内的平均回收率为88.53%~119.03%,RSD为1.25%~14.70%(n=3);方法定量限为0.2~1 μg·kg-1。结论 本方法专属性强、灵敏度高、测定结果准确,可用于中药材中16种典型多环芳烃的残留检测。
Abstract
OBJECTIVE To develop a GC-MS/MS method for the determination of the residues of 16 polycyclic aromatic hydrocarbons (PAHs) in Chinese herbal medicines. METHODS Using isotope as internal standard, the sample was extracted by ethyl acetate and purified by solid phase extraction on C18 cartridges. GC-MS/MS method was used for the assay, with analyte protectants added to counteract the matrix effect. The chromatographic column was DB-5ms(0.25 mm×30 m,0.25 μm) with temperature programming and MRM detection. RESULTS The calibration curves for the 16 kinds of typical PAHs were linear in the range of 1-100 ng·mL-1. The average recovery rate was 88.53%-119.03% in the range of 1-25 μg·kg-1 with RSDs of 1.25%-14.70%(n=3). The LOQs were 0.2-1 μg·kg-1. CONCLUSION This method is specific, sensitive, accurate and can be used for residue detection of 16 typical kinds of PAHs in Chinese herbal medicines.
关键词
多环芳烃 /
中药材 /
气相色谱串联质谱法 /
同位素内标 /
分析保护剂
{{custom_keyword}} /
Key words
polycyclic aromatic hydrocarbon /
traditional Chinese medicine /
gas chromatography-tandem mass spectrometry /
isotope internal standard /
analyte protectants
{{custom_keyword}} /
中图分类号：
R917
{{custom_clc.code}}
({{custom_clc.text}})
{{custom_sec.title}}
{{custom_sec.title}}
{{custom_sec.content}}
参考文献
[1] KOU Y J. Determination of benzo(α) pyrene inmultifarious natural P E by HPLC-FLD. West China J Pharm Sci(华西药学杂志),2008,23(2): 197-198.
[2] YU W S, YU W H, SHI R D, et al. Content of 16 kinds of polycyclic aromatic hydrocarbons in edible oils . Chin J Health Lab Technol (中国卫生检验杂志),2013,23(7):1793-1795.
[3] QIAN H O, WANG M J, HU J W,et al. Simultaneous determination of fifteen polycyclic aromatic hydrocarbons in plant oil by high performance liquid chromatography . Chin J Food Hygiene(中国食品卫生杂志),2013,25(5):434-437.
[4] GUO M M, WU H Y, YANG F,et al. Determination of 16 polycyclic aromatic hydrocarbons in fishery products by improved QuEChERS-high performance liquid chromatography. Environ Chem(环境化学),2013,32(6):1025-1031.
[5] HAN Y, LU Y, YANG Y, et al. Determination of four kinds of polycyclic aromatic hydrocarbon metabolites in human urine by liquid chromatography-tandem mass spectrometry. J Environ Health (环境与健康杂志),2012,29(10):933-936.
[6] NUNO R,SILVIA L,DAMIA B, et al. Microwave-assisted extraction and ultrasonic extraction to determine polycyclic aromatic hydrocarbons in needles andbark of Pinus pinaster Ait. and Pinus pinea L.by GC-MS. Talanta, 2009,77(11):1120-1128.
[7] WANG N, KONG D Y.Simultaneous determination of pesticides, polycyclic aromatic hydrocarbons, polychlorinated biphenyls and phthalate esters in human adipose tissue by gas chromatography-tandem mass spectrometry. J Chromatography B, 2012, 898(1):38-52.
[8] MEUDEC A, DUSSAUZE J, JOURDIN M, et al. Gas chromatographic-mass spectrometric method for polycyclic aromatic hydrocarbon analysis in plant biota. J Chromatography A, 2006, 1108(1):240-247.
[9] BO H B. Determination and confirmation of benzopyrene in Chinese herbal medicines Rehmanniae Radix Praeparata by gas chromatography-triple quadrupole tandem mass spectrometry. Chin J Pharm Anal(药物分析杂志),2013,33(12):2119-2122.
[10]WANG Y, JIN H Y, MA S C, et al. Determination of 195 pesticide residues in Chinese herbs by gas chromatography-mass spectrometry using analyte protectants.J Chromatography A,2011,1218(2):334-342.
{{custom_fnGroup.title_cn}}
脚注
{{custom_fn.content}}
基金
“重大新药创制”国家科技重大专项课题“中药质量安全检测和风险控制技术平台”(2014ZX09304307-002)
{{custom_fund}}
PDF(932 KB)
