| Traditional Chinese herb is widely applied with many medical values, but it has been polluted with pesticides which have been abused in Chinese herbal planting. Gas chromatography(GC) and gas chromatography coupled to tandem mass spectrometry(GC-MS/MS) are popular dection instruments which have limited in the dection of pesticides. In recent years, the new type pesticides are widely used and popularized in agriculture. Liquid chromatography coupled to tandem mass spectrometry(LC-MS/MS) stands out in the dection of pesticides with many advantages. Ultra-performance liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS) has improvements on LC-MS/MS. It provides higher analytical efficiency and sensitivity which be designed for accurate quantification. Therefore, this study chose different texture of traditional Chinese patent medicine(Semifluid extract of deer foetus and Shengmaiyin) and traditional Chinese herb(Hedyotis diffusa, Rosa rugosa Thunb, Ophiopogon japonicas and Codonopis pilosula) as sample matrices, UPLC-MS/MS as a dection method to determine the multi-residue of pesticides in traditional Chinese medicine.In this study, a QuEChERS-UPLC-MS/MS method was performed to analyze the multi-residue of neonicotinoid insecticides in Hedyotis diffusa and Semifluid extract of deer foetus. UPLC-MS/MS was used for the quantification and confirmation of five compounds. The extraction, clean-up, UPLC separation and MS/MS parameters were especially optimized. The low limits of detection(LODs) of five insecticides ranged from 0.04 to 0.81 μg/kg,the limits of quantification(LOQs) were between 0.13-2.68 μg/kg. The recoveries of the five insecticides ranged from 80.2% to 105.4% with RSDR of 1.7%-10.6%. The results demonstrated that the method is an accurate approach to make an analysis of neonicotinoids in traditional Chinese medicine.A method for the determination of multi-pesticides was developed using a QuEChERS-UPLC-MS/MS in Rosa rugosa Thunb. Samples were extracted by 0.1% acetic acid-acetonitrile, and then salting-out by adding NaCl and anhydrous MgSO4. After that, the extract was removed to a tube which contained primary secondary amine(PSA), graphitized carbon black(GCB) and anhydrous MgSO4 to purify. UPLC-MS/MS in the multiple reaction monitoring(MRM) mode was used for the confirmation and determination of 19 target compounds. An external matrix-matched calibration method was used to obtain precise quantification. The correlation coefficient was higher than 0.9934 in the linear range of 1-100 μg/kg. The recoveries 77.8%-110.9% of target compounds were obtained in different spiked levels(1, 5 and 10 μg/kg). LODs and LOQs for 19 compounds were in the ranges of 0.023-0.26 μg/kg and 0.078-0.87 μg/kg, respectively. This method meets the requirements of the analysis of multiple classes of pesticide.This paper developed an analytical method which based on ultrasonic assisted-QuEChERS-DLLME-UPLC-MS/MS for the determination of 19 commonly used pesticides in Shengmaiyin and its resulting crude drugs(Codonopis pilosula and Ophiopogon japonicas). The target compounds were qualitatively and quantitatively studied via UPLC-MS/MS operated in MRM mode. The correlation coefficient was higher than 0.9935 in the linear range of each pesticide. Recoveries of the 19 compounds from different fortified samples ranged between 80.9% and 107.5% with RSDR below 17.7%. LODs and LOQs for 19 compounds were in the ranges of 0.0022-0.24 μg/kg and 0.0075-0.81 μg/kg, respectively. Recovery, LODs and LOQs of the DLLME method were compared with the routine QuEChERS method, and the results showed that the proposed method is very simple, rapid and sensitive. This makes it a more applicable method for monitoring multiple classes of pesticides in traditional Chinese medicine. |
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