Dissipation and residue of flonicamid in cucumber,apple and soil under field conditions

A method based on QuEChERS-like extraction and UPLC-ESI-MS/MS for the analysis of flonicamid was established. The samples were extracted by acetonitrile–methanol mixture and were purified using PSA. At fortification levels of 0.01, 0.1 and 0.5 mg/kg in cucumber, apple and soil, recoveries ranged from 71.5 to 106.0% with relative standard deviation (RSD) of 2.6–9.9%. The limit of quantification (LOQ) was 0.003 mg/kg for cucumber, apple and soil. This study also investigates the dissipation of flonicamid in cucumber, apple and soil. The dissipation half-lives of flonicamid in cucumber, apple and soil were 3.0–4.9 days, 5.1–6.1 days and 10.3–14.2 days, respectively. The final residues of flonicamid ranged from 0.029 to 0.295 mg/kg in cucumbers, <0.01–0.174 mg/kg in apples and <0.01–0.172 mg/kg in soil, respectively. The observed low residual levels of flonicamid suggest that the cucumber and apple are safe when applied at the recommended dosage.     

Determination of 10 pesticides,newly registered in Egypt,using modified QuEChERS method in combination with gas and liquid chromatography coupled with tandem mass spectrometric detection

The analysis of pesticide residues in food is currently an increasingly important task. In this work, a rapid and sensitive protocol has been developed for the determination of ametoctradin, amisulbrom, bromoxynil-octanoate, chlorantraniliprole, cyhalofop-butyl, hymexazol, metaldehyde, prodiamine (dithiopyr), sulcotrione and tolfenpyrad. The extraction was done using the citrate buffer acetonitrile-based QuEChERS (quick, easy, cheap, effective, rugged and safe) sample preparation technique. Acetonitrile extracts were directly injected into the liquid chromatography-tandem mass spectrometry system, and solvent exchange was used prior to the injection in the gas chromatography system. Different exchange solvents were evaluated and a mixture of n-hexane:acetone (9:1) was chosen. Matrix effects were evaluated and a relation between the signal suppression/enhancement and the co-extracted matrix was established. The validation study was carried out on cucumber, banana and lemon matrices following SANTE/11813/2017 of the European quality control guidelines. The precision and trueness of the method were determined from recovery experiments on six replicates of spiked blank samples at 0.01, 0.05, and 0.1 mg/kg for each commodity. The range of the obtained recoveries was 70–111%, with RSD values of <18% for all the tested concentrations. The only exception was hymexazol at 0.01 mg/kg in banana and cucumber.     

Residues of four triazole fungicides in tobacco leaves under field condition and during curing

Residues of four triazole fungicides (triadimefon, myclobutanil, tebuconazole and difenoconazole) in tobacco leaves under field condition and during curing were investigated. Following extraction with acetonitrile, the samples were cleaned up by a Florisil solid phase extraction column, and then determined by gas chromatography–mass spectrometry in selected ion monitoring mode. The average recoveries of the four triazole fungicides were found in the range of 82.7–97.3% with relative standard deviations of 1.1–4.6% in green and cured tobacco leaves. The residues of triadimefon, myclobutanil, tebuconazole and difenoconazole in Shandong, Sichuan, Yunnan, Liaoning and Jiangxi were found in the range of 0.02–0.32 mg/kg, 0.41–4.93 mg/kg, 0.37–9.84 mg/kg and 0.25–4.85 mg/kg in cured tobacco leaves when measured 14 days after the last application. The residue levels of the four triazole fungicides in most cured tobacco samples were lower than that in green tobacco samples, indicating that high temperature degradation surpassed dehydration concentration during the curing process.     

Multiresidue analysis of pesticides with hydrolyzable functionality in cooked vegetables by liquid chromatography tandem mass spectrometry

It would be preferable for pesticide residues substituted by hydrolyzable functionality to be analyzed after cooking because their structures are apt to degrade during boiling and/or heating. A liquid chromatography–tandem mass spectrometry (LC‐MS/MS) method for the quantitative determination of 44 pesticide residues with hydrolyzable functional group in five typical vegetable widely consumed in Republic of Korea is described. The sample clean‐up was carried out according to the method of Food Code No. 83 established by the Korea Food and Drug Administration (KFDA). Zorbox XDB‐C₁₈ column was selected for the analysis because of the best peak separation. The LC mobile phase consisted of water and 5 mm methanolic ammonium formate, which resulted in a peak shape with good symmetry at each run. Tandem mass spectroscopic (MS/MS) experiments were performed in ESI positive mode and the multiple reaction monitoring modes. A conventional matrix effect was modified to more comprehensive form 100γ_ij (%). A high matrix effect (相似文献   

Use of a Headspace Solid-Phase Microextraction-Based Methodology Followed by Gas Chromatography–Tandem Mass Spectrometry for Pesticide Multiresidue Determination in Teas

This study reports on the development of a fast and efficient method based on headspace solid-phase microextraction (HS-SPME) coupled to gas chromatography–tandem mass spectrometry (GC–MS/MS) for simultaneous analysis of 128 volatile or semi-volatile pesticide residues belonging to nine classes of pesticides. The important factors related to HS-SPME performance were optimized; these factors include fiber types, water volume, ion strength, extraction temperature, and extraction time. The best extraction conditions include a PDMS/DVB fiber, and analytes were extracted at 90 °C for 60 min from 1 g of tea added to 5 mL of 0.2 g mL^?1 NaCl solution. The methodology was validated using tea samples spiked with pesticides at three concentration levels (10, 50, and 100 μg kg^?1). In green tea, oolong tea, black tea, and puer tea, 82.8, 88.3, 79.7, and 84.3% of the targeted pesticides meet recoveries ranging from 70 to 120% with a relative standard deviation of?≤?20%, respectively, when spiked at a level of 10 μg kg^?1. Limits of quantification in this method for most of the pesticides were 1 or 5 μg kg^?1, which are far below their maximum residue limits prescribed by EU. The optimized method was employed to analyze 30 commercial samples obtained from local markets; 17 pesticide residues were detected at concentrations of 2–452 μg kg^?1. Chlorpyrifos was the most detected pesticide in 80% of the samples, and the highest concentration of dicofol (452 μg kg^?1) was found in a puer tea. This is the first time to find that the optimized extraction temperature for pesticide residues is 90 °C, which is much higher than other reported HS-SPME extraction conditions in tea samples. This developed method could be used to screen over one hundred volatile or semi-volatile pesticide residues which belong to multiple classes in tea samples, and it is an accurate and reliable technique.     

Determination of cyantraniliprole and its major metabolite residues in vegetable and soil using ultra-performance liquid chromatography/tandem mass spectrometry

A rapid, highly sensitive and selective method was developed for the determination of the cyantraniliprole and its major metabolite J9Z38 in cucumber, tomato and soil by ultra‐performance liquid chromatography–tandem mass spectrometry (UPLC‐MS/MS). Target compounds were extracted with acetonitrile and an aliquot cleaned with primary and secondary amine. Two pairs of precursor product ion transitions for cyantraniliprole and J9Z38 were measured and evaluated. Average recoveries for cucumber, tomato and soil at three levels (10, 50 and 100 µg/kg) ranged from 74.7 to 96.2% with intra‐day relative standard deviation (RSD) of 2.6–15.1% and inter‐day RSD of 3.4–13.3%. The limit of quantitation for cyantraniliprole and J9Z38 were determined to be 5 and 10 µg/kg in samples (cucumber, tomato and soil), respectively. This method was used to determine the cyantraniliprole and J9Z38 residues in real cucumber, tomato and soil samples for studies on their dissipation. The trial results showed that the half‐lives of cyantraniliprole obtained after treatments were 2.2, 2.8 and 9.5 days in cucumber, tomato and soil in Zhejiang, respectively, and that the average levels of cyantraniliprole and J9Z38 residues in cucumber and tomato were all <0.01 mg/kg with the interval of 10 days after treatment. Copyright © 2011 John Wiley & Sons, Ltd.     

Validation of short run time LC-ESI (+) MS/MS method for determination of twenty recommended pesticide residues in food based on QuEChERS extraction technique

Food is expected to contain pesticide residues that might have many problems due to their toxicities for human and animals. So, it is very important to detect and quantify the pesticides contamination levels to increase food safety for the human. The target of our study is to analyse a 20 new pesticides including different pesticide classes such as 1 acaricide, 3 fungicides, 2 plant growth regulators, 11 herbicides, 1 insecticide, 1 rodenticide, and 1 metabolite which were selected according to their modern application in the Egyptian agriculture as well as the recommendation of the Egyptian Agriculture Pesticides Committee (APC). The research is focused on the method validation for the routine analysis of the targeted pesticide residues according to the European SANTE/11,813/2017 guideline. The validation was carried out by fortifying of three levels at 0.01, 0.05 and 0.1 mg/kg in four blank matrices: apple, green beans, fennel seeds and rice which represent different classes of food. The most common citrate buffered QuEChERS extraction method and liquid chromatography coupled with triple quadrupole mass spectrometry (LC-MS/MS) device were used. The mass spectrometer was operated in the positive electrospray ionisation ESI (+) mode and the non-scheduled multiple reactions monitoring (MRM) method in a short run time of 16.0 min. The limits of quantifications (LOQs) for all pesticides ranged between 0.01 and 0.05 mg/kg. Good linearity of the method was in the concentration range 0.001–0.5 μg/ml with acceptable correlation coefficients (r²) ≥ 0.99 for all analytes. The average recoveries for all the target pesticide residues were in the range of 70–120% with relative standard deviations RSDs ≤ 20%. The matrix effect was compensated by using the standard addition method. This short run time LC ESI (+) MS/MS Method may help laboratories which deal with the routine pesticide residues analysis in different food samples.     

Pyraflufen-ethyl residues in soil by solid phase extraction and high-performance liquid chromatography with UV detection.

Solid-phase extraction (SPE) procedure for cleanup followed by HPLC-UV method has been investigated for the determination of pyraflufen-ethyl residues in soil. The pesticide is extracted from the sample with acetone-water (80:20, v/v) and the extract is loaded onto an octadecyl (C(18)) column. The pesticide is eluted with acetonitrile and determined by HPLC with a UV detector. Using an acetone-water extraction followed by a C(18) cleanup, this method is characterized by recovery >90.1%, precision <5.8% RSD and sensitivity of 0.01 mg/kg. The proposed method has been successfully employed for the determination of the degradation dynamics of pyraflufen-ethyl in four agricultural soil samples under laboratory conditions.     

Pesticide residue determination in vegetables from western China applying gas chromatography with mass spectrometry

In this study,an effort has been made to evaluate the pesticide residues in vegetables from western China. Fifty‐one pesticides, including organophosphorus, organochlorine, carbamate and pyrethroid, were detected in 369 commonly used vegetables by GC‐MS. Concentrations of organophosphorus pesticides were detected ranging from 0.0008 to 18.8200 mg/kg, among which organophosphorus pesticide concentrations exceeded their maximum residue levels (MRLs) in five samples. Carbamate and organochlorine pesticides were determined to have concentrations in the range of 0.0012–0.7928 mg/kg. The residual concentrations of carbamate pesticides in six samples and organochlorine pesticides in four samples exceeded their MRLs. The residual concentrations of five pyrethroid pesticides were within the range of 0.0016–6.0827 mg/kg and the pyrethroid residues in two samples exceeded their MRLs. The results revealed that pesticide residues in 70.73% of the vegetables samples were not detected, while in the rest of vegetables there were one or more pesticide residues and some even exceeded their MRLs, which would threaten the health of consumers. Our work provides significant information for the food safety regulations to control the excessive use of some pesticides on those kinds of vegetables from western China. Copyright © 2016 John Wiley & Sons, Ltd.     

Simultaneous determination of chlorpyrifos and 3,5,6-trichloro-2-pyridinol in duck muscle by modified QuEChERS coupled to gas chromatography tandem mass spectrometry (GC-MS/MS)

A rapid, specific, and sensitive method based on modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) coupled to gas chromatography tandem mass spectrometry (GC-MS/MS) was developed and validated for simultaneous determination of chlorpyrifos (CP) and its metabolite 3,5,6-trichloro-2-pyridinol (TCP) in duck muscle. The residues of CP and TCP were extracted by acidified acetonitrile. The fat layer of the extract was removed under ?20 °C, then the organic layer was evaporated. The analytes were derivatized by N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) and cleaned up by a mixture of 150 mg MgSO₄, 25 mg graphitized carbon black (GCB), and 50 mg N-propylethylenediamine (PSA) to remove interference. The final extract was analyzed by GC-MS/MS. Recovery values at the spiking concentrations ranged from 86.2 to 92.3 % for CP and from 74.8 to 81.8 % for TCP, with relative standard deviations (RSDs) lower than 9.5 and 12.3, respectively. The correlation coefficients of CP (from 2 to 2,000 μg/kg) and TCP (from 1 to 1,000 μg/kg) were equal to or higher than 0.998. The limits of detection (LODs) were 0.3 and 0.15 μg/kg, and the limits of quantification (LOQs) were 1.0 and 0.5 μg/kg for CP and TCP in duck muscle, respectively. The average intra- and inter-day accuracy ranged from 84.6 to 91.2 % for CP and 75.6 to 82.3 % for TCP, and the intra- and inter-day precisions were from 5.8 to 8.2 % for CP and 6.5 to 11.9 % for TCP. Furthermore, the CP and TCP residues in duck muscle samples were detected for dietary risk assessment using the validated method.

Stability of Parathion-Methyl,Methiocarb, DDT and 2,4-D in Solid-Phase Extraction Precolumns Packed with a Polymeric Reversed Phase

Abstract

The stability of parathion-methyl, methiocarb, DDT and 2,4-D, adsorbed on the polymeric PLRP-S phase packed in small stainless steel precolumns was examined, with a view to propose the use of these precolumns as alternative means for the transport of water samples. First, water samples spiked with the studied pesticide at low μg/l concentration levels were extracted and preconcentrated in the precolumns, using appropriate conditions for a total recovery. Then, the precolumns were stored at room temperature (15—20°C) or at 35°C for different time periods. At the end of the respective period each precolumn was coupled to an HPLC column via a switching valve and was on-line analyzed by reversed phase chromatography with UV detection. The four pesticide recoveries after one week in the precolumn at room temperature were higher than 90%. The same was true at 35°C except for DDT, which suffered a 30% degradation in one week. Further studies showed that DDT and parathion-methyl were stable at least for five weeks in precolumns stored at room temperature. Methiocarb also was stable for this period but storing the precolumns at 4°C.     

Development and Validation of a Dispersive Solid Phase Extraction Liquid Chromatography Mass Spectrometry Method with Electrospray Ionization for the Determination of Multiclass Pesticides and Metabolites in Meat and Milk

A dispersive solid phase extraction–liquid chromatography tandem mass spectrometry method with electrospray ionization was validated in food of animal origin for the determination of multiclass pesticide residues and their metabolites. A simple and low-cost sample preparation procedure using freezing as the clean-up step was used to identify and quantify analytes belonging to 39 different chemical classes in meat and milk matrices. Mean recoveries in the range of 70–120% with relative standard deviations <10% were obtained for the majority of the analytes. The limit of quantification of the method was 10 µg/kg. The matrix effects were statistically evaluated and the quantification of the analytes was conducted using calibration curves constructed with matrix matched calibration standards covering concentrations from 5 to 200 µg/kg. The proposed method was applied in 86 samples of animal origin taken from the Greek market, two of which were found positive for pesticides.     

Development of GC–MS/MS method for environmental monitoring of 49 pesticide residues in food commodities in Al-Rass,Al-Qassim region,Saudi Arabia

The harmful effects of pesticide residues are a threat to our health. Therefore, the current study aimed to validate a simple method for the determination of pesticide residues in commonly consumed fruits and vegetables from Al-Rass, Al-Qassim region, Saudi Arabia. A total of 1430 samples were collected from a local market and then analyzed for monitoring of 49 pesticide residues. A quick, easy, cheap, effective, rugged, and safe (QuEChERS) multi-residue extraction method followed by gas chromatography equipped with triple-quadrupole mass spectrometry (GC–MS/MS) was successfully implemented. This 17-min-run analytical method detects and quantifies pesticide residues with acceptable validation performance parameters in terms of sensitivity, selectivity, linearity, the limit of quantification, accuracy, and precision. The linear range of the calibration curves ranged from 10 to 300 µg/L, all the pesticide LODs ranged from 0.0005 to 0.0024 mg/kg, and the pesticide LOQs ranged from 0.0011 to 0.0047 mg/kg. The recovery values at the three fortification levels ranged from 78 % to 107 %, and the precision values (expressed as RSD%) were less than 20 % for all of the investigated analytes. The results showed that 138 (9.65 %) of the analyzed samples were contaminated with pesticide residues, 40 (2.80 %) of the analyzed samples exceeded the maximum residue limit (MRL) of the European Commission regulations (EC) for pesticides residues, 98 (6.85 %) of the analyzed samples were contaminated with residues below the MRL, and 1292 (90.35 %) of the analyzed samples were pesticide residue-free. Coriander contained the highest percentage (46.88 %) of pesticide residues, particularly tetradifon that representing 18.75 % noncompliance with the MRL, followed by parsley, with 20.59 % pesticide residues (10.29 % non-compliance). Multiple pesticide residues were observed most frequently in tomatoes and dates which were contaminated with buprofezin and ethion respectively.     

Synthesis,characterization and thermal stability of new dumbbell-shaped isobutyl-substituted POSSs linked by aromatic bridges

Five new dumbbell-shaped polyhedral oligomeric silsesquioxanes (POSSs), in which two identical silicon cages R₇(SiO_1.5)₈ (with R = isobutyl), linked to various aromatic bridges (Ar, Ar–Ar, Ar–O–Ar, Ar–S–Ar and Ar–SO₂–Ar, where Ar = p-C₆H₄) were prepared through a literature method opportunely modified by us to make easier preparation and increase yield, which was higher than 70 % in all cases. The obtained products were the expected ones, as supported by the results of elemental analysis and ¹H NMR spectra. Their resistance to the thermal degradation in both flowing nitrogen and static air atmosphere was checked by degrading samples at 10 °C min^?1 and determining temperatures at 5 % mass loss (T _5%) and residues at 700 °C. The T _5% values in air were lower than the corresponding ones in nitrogen, but the trend among the various POSSs investigated was the same in both used atmospheres, with the most high value for the compound having the Ar–O–Ar aromatic bridge. The residues at 700 °C in air of the compounds having not hetero-atoms (O or S) in the aromatic bridge were higher than those in nitrogen, whilst no substantial difference was observed for the other ones.     

Determination of pesticide residues in peaches by using gas chromatography and mass spectrometric detection

ABSTRACT

A multi-residue method using selected ion monitoring mode GC-MSD has been developed for the quantitative analysis of 30 widely used pesticides in fresh peaches produced in Swat Malakand, Pakistan. The planned methodology involved a sample extraction procedure using liquid-liquid partition with acetonitrile followed by a clean-up step based on solid-phase extraction (SPE). Method validation was performed in accordance with European Union guidelines. The European Union criteria (recovery 70–120%, RSD <20%) were met for majority of pesticides. For most of the pesticides, signal-to-noise ratios were good and background-corrected mass spectra often contained sufficient diagnostic to enable identity and confirmation. The limits of quantification (LOQs) were in the range 0.01–1.0 mg/kg. The above method was successfully applied to the analysis of peach samples (n = 30) from the field. Pesticide concentration in real peach samples was compared with the maximum residue levels (MRLs). Pesticide residues were detected in 73% of the peach samples. Most frequent residues were metalaxyl, α-cypermethrin, azoxystrobin, dimethoate, tebuconazol, λ-cyhalothrin and spiromesifin in peach samples.     

Multiresidue method for the determination of residues of 251 pesticides in fruits and vegetables by gas chromatography/mass spectrometry and liquid chromatography with fluorescence detection

A method is described for the determination of 251 pesticide and degradation product residues in fruit and vegetable samples. Extraction of the sample with acetonitrile is followed by a salting-out step. Co-extractives are removed by passing a portion of the acetonitrile extract through an octadecyl (C18) solid-phase extraction cleanup cartridge and then, in a second cleanup, through a carbon cartridge coupled to an amino propyl cartridge. Determination is by gas chromatography with mass-selective detection in the selected-ion monitoring mode, and by liquid chromatography with post-column reaction and fluorescence detection for N-methyl carbamates. The method has been used for analysis of various fruits and vegetables, such as apple, banana, cabbage, carrot, cucumber, lettuce, orange, pear, pepper, and pineapple. Limits of detection range between 0.02 and 1.0 mg/kg for most compounds. Over 80% of the compounds have a limit of detection of < or = 0.04 mg/kg.     

Behaviour of selected pesticide residues in blackcurrants (<Emphasis Type="Italic">Ribes nigrum</Emphasis>) during technological processing monitored by liquid-chromatography tandem mass spectrometry

In this experiment, the behaviour of ten pesticides on field-sprayed blackcurrants (Ribes nigrum) after washing, juicing and cooking was investigated. The concentration level changes in two acaricides (fenazaquin, propargite), three insecticides (alpha-cypermethrin, deltamethrin and lambdacyhalothrin) and five fungicides (boscalid, bupirimate, difenoconazole, pyraclostrobin, thiophanate-methyl) were quantified. Analysis was carried out using the QuEChERS method followed by chromatographic analysis based on LC-MS/MS. The matrix effects ranged from —(17.4 ± 8.1) % to (15.9 ± 7.8) %. The limits of detection and limits of quantification were 0.003 mg kg^?1 and 0.01 mg kg^?1, respectively. The mean recoveries of the analytes ranged between 71 % and 109 %. The processing factors of all the blackcurrant products were determined. Washing reduced the pesticide residues up to 71 %. Juicing significantly reduced all the pesticide residues (processing factors (PFs) ranged 0.14–0.47). Cooking resulted in a decrease in residues up to 82 %. The residue levels of alpha-cypermethrin, deltamethrin and lambda-cyhalothrin in blackcurrant jam increased, and PFs > 1 were noted as PF = 1.38, 1.66 and 1.04, respectively. Cluster analysis was performed to find any similarity in the behaviour of pesticides after processing. The results confirmed that solubility, polarity and mode of action could be used to explain differences in the behaviour of pesticides.     

Retrogradation characteristics of high hydrostatic pressure processed corn and wheat starch

High hydrostatic pressure (HHP) has been investigated as an alternative to thermal processing for food preservation. HHP has been known to affect high molecular weight polymers causing phase change. Starch is gelatinized at a pressure on the order of 600–700 MPa, at 25 °C. Gelatinized starch recrystallizes during storage affecting the texture and shelf life of food products. The effect of HHP processing on the crystallization of starches from different botanical origins during storage at 4 and 23 °C was investigated. Crystallization kinetics of HHP treated wheat and corn starch gels were compared using DSC. The effect of crystallization on structure was evaluated in terms of storage modulus. The rate of retrogradation depended on the storage temperature (23 °C and 4 °C) and the botanical origin of the starch. The least crystallization was observed in HHP treated wheat starch stored at 23 °C. The storage modulus increased with crystallization of starch.     

An internal surface reversed phase column for the effective removal of humic acid interferences in the trace analysis of mecoprop in soils with coupled-column RPLC-UV

In the development of a screening method for the determination of residues of mecoprop in soils involving coupled-column RPLC-UV (228 nm) the cleanup performance of a 5 μm GFF-II internal surface reversed phase (ISRP, Pinkerton) analytical column (50 × 4.6 mm I.D.) as a first column was investigated. In comparison to an analytical C18 column the ISRP column substantially improved the separation between acidic analyte and co-extracted humic substances. Under the selected coupled-column conditions soil extracts obtained after hydrolysis with an aqueous alkaline solution, acidifying and centrifugation could be analyzed directly allowing the determination of mecoprop in soils to a level of about 0.02 mg/kg. A rapid concentration step on a 100 mg C18 solid phase extraction (SPE) cartridge was adopted into the procedure providing a limit of detection (S/N = 3) of 0.01 mg/kg of mecoprop in soil. The method was validated by analyzing freshly spiked soil samples and samples with aged residues. In case of freshly spiked samples the overall recovery was 87% (n = 18, spiked level 0.02–8.0 mg/kg) with a repeatability of 6.8% and a reproducibility of 8.3%. No significant decrease of the recovery was observed for samples with aged residues (n = 15, spiked level 0.1 and 8.0 mg/kg) during a storage of 29 days in the refrigerator at about 4?°C; a storage of 67 days provided a mean recovery of 76% (n = 14, spiked level 8.0 mg/kg).     

微波辅助提取-气相色谱法同时测定中草药中有机磷和氨基甲酸酯农药残留

建立了中草药中有机磷和氨基甲酸酯类农药同时检测的气相色谱分析新方法.中药材试样依据正交实验的优化条件,用正己烷-丙酮(1∶4,V∶V)混合提取剂进行微波辅助提取,经弗罗里硅土和中性氧化铝混合层析柱净化后,采用HP-5毛细管柱分离,氮磷检测器同时检测中草药中15种有机磷和6种氨基甲酸酯类农药残留量.21种农药在0.01～1.0 mg/L的浓度范围内线性良好,线性相关系数为0.9950～1.000,检出限为0.002～0.01 mg/L.在0.05、0.2、0.5 mg/kg三个添加水平的平均回收率分别为75.11%～128.57%、75.85%～120.71%和76.43%～117.25%,相对标准偏差分别为 3.10%～10.58%、5.27%～9.94%和4.03%～9.03%.方法用于中草药中有机磷和氨基甲酸酯类农药残留的同时检测,结果良好.