| Objective: A new gas chromatography method coupled with ultrasound-assisted extraction and solid-phase microextraction（UAE-SPME-GC）was established for rapid analysis of pesticides residue in traditional Chinese medicines. Compared with UAE-SPME-GC, pesticides residue were also analyzed by Chinese Pharmacopoeia（2010） method. Heavy metals in traditional Chinese medicines were also detected in this experiment. Methods:（1） Flos Lonicerae Japonicae was an optimization object. Before analyzed by GC, the sample was extracted by organic solvent and ultrasound, then enriched by SPME.（2） Pesticides residue were also detected by the method of Chinese Pharmacopoeia（2010）.（3）According to the second method in appendix IX B of Chinese Pharmacopoeia（2010）Pb, Cd, Hg, As and Cu were detected. Results:（1） In the method of UAE-SPME-GC,under the optimized conditions, linearities of 8 kinds of OCPs ranged from 0.5 μg·L-1to 20 μg·L-1 were all with good correlation coefficients. The spiked recoveries ranged from 70.4% to 119.8% and relative standard deviations（RSD） ranged from8.9% to 14.1%. The detection limits were from 0.017 μg·L-1 to 0.38 μg·L-1. The linearities of 7 kinds of OPPs ranged from 5 μg·L-1 to 100 μg·L-1 and 3 kinds of pyrethroid pesticides ranged from 2.5 μg·L-1 to 50 μg·L-1 were all with good correlation coefficients. The spiked recoveries ranged from 85.6% to 112.7% and relative standard deviation（RSD） ranged from3.2% to 9.8%. The detection limits were from 0.02 μg·L-1 to 0.33 μg·L-1.（2） In the method of Chinese Pharmacopoeia（2010）, linearities of OCPs ranged from 5 μg·L-1 to 100 μg·L-1 were all with good correlation coefficients. The spiked recoveries ranged from 86.1% to 115.0% and relative standard deviations（RSD） ranged from 1.2% to 5.1%. The detection limits were from 0.55 μg·L-1 to 1.79 μg·L-1. linearities of organophosphorus pesticides ranged from 10 μg·L-1 to 500 μg·L-1 and pyrethroid pesticides ranged from 5 μg·L-1to 250 μg·L-1 were all with good correlation coefficients. The spiked recoveries ranged from 83.1% to 105.3% and relative standard deviations（RSD） ranged from1.9% to 4.8%. The detection limits were from 0.53 μg·L-1 to 1.75 μg·L-1.（3） In the detection of heavy metals, the detection limits were from 0.005 μg·L-1 to 0.039μg·L-1. The recoveries ranged from 94.9% to 101.3% and relative standard deviations（RSD） ranged from2.5% to 6.7%. Conclusion: The experiment demonstrated that SPME has higher sensitivity than Chinese Pharmacopoeia（2010）.As a new technology for pre-treatment, SPME was a kind of extraction,concentration and sample injection. UAE-SPME-GC was a convenient,environmental, rapid method with enrichment and high sensitivity. The resaults of heavy metals detection show that these traditional Chinese medicines are eligible with the low content of heavy metals. |
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