摘要
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,0.25μm),程序升温,MRM模式检测。结果 16种典型多环芳烃在1~100ng·m L-1内呈线性关系;在1~25μg·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0.2~1μg·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。
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- 100ng·m L- 1. The average recovery rate was 88. 53%- 119. 03% in the range of 1- 25 μg·kg- 1with 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.
出处
《中国药学杂志》
CAS
CSCD
北大核心
2015年第2期115-119,共5页
Chinese Pharmaceutical Journal
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)
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
polycyclic aromatic hydrocarbon
traditional Chinese medicine
gas chromatography-tandem mass spectrometry
isotope internal standard
analyte protectants
