分散液-液微萃取-气相色谱法快速检测番茄中3种拟除虫菊酯类农药

建立了快速(quick)、简单(easy)、便宜(cheap)、有效(effective)、可靠(rugged)和安全(safe)(QuEChERS)的分散液-液微萃取(DLLME)-气相色谱快速测定番茄中拟除虫菊酯类农药残留的方法。样品经乙腈提取,N-丙基乙二胺(PSA)净化,采用DLLME富集,用气相色谱法分析。考察了联苯菊酯、甲氰菊酯和氟氰菊酯在番茄中的残留测定,同时考察了萃取剂种类与体积、分散剂体积以及萃取时间等因素对萃取效率的影响,以40 μL氯仿为萃取剂,1000 μL乙腈为分散剂,萃取时间为60 s。结果表明: 3种拟除虫菊酯类农药在番茄中的检出限分别为0.5、0.5、0.3 μg/kg。在1、10和50 μg/kg添加水平下,联苯菊酯、甲氰菊酯和氟氰菊酯在番茄中的平均回收率分别为89%～109%、92.5%～105%和90%～108%,相对标准偏差分别为2.5%～7.6%、2.8%～5.7%、3.8%～9.1%。该方法简便、快速、安全、价格低廉,重现性好,可用于番茄中拟除虫菊酯类农药的快速检测。     

Combination of a modified quick,easy, cheap,efficient, rugged,and safe extraction method with a deep eutectic solvent based microwave‐assisted dispersive liquid–liquid microextraction: Application in extraction and preconcentration of multiclass pesticide residues in tomato samples

In this study, a new two–step extraction procedure based on the combination of a modified quick, easy, cheap, effective, rugged, and safe extraction method with a deep eutectic solvent based microwave‐assisted dispersive liquid–liquid microextraction has been developed for the extraction of multiclass pesticides in tomato samples before their analysis by gas chromatography with flame ionization detection. In this method, initially, an aliquot of tomato is crushed and diluted with deionized water. The mixture is then passed through a filter paper and its residue and aqueous phase are separated. Afterwards, acetonitrile as an extraction/disperser solvent is passed through the filter paper containing the refuse. The analytes remained in the refuse are extracted into the acetonitrile and then the obtained extract is mixed with a deep eutectic solvent. The obtained mixture is injected into the tomato juice and placed in a microwave oven for 15 s. Consequently, a cloudy state is formed and the extractant containing the analytes are sedimented at the bottom of the tube after centrifugation. Finally, 1 μL of the sedimented phase is removed and injected into the separation system. Under the optimum conditions, limits of detection and quantification were in the ranges of 0.42–0.74 and 1.4–2.5 ng/g, respectively.     

Simultaneous extraction and determination of antibiotics in soils using a method based on quick,easy, cheap,effective, rugged,and safe extraction and liquid chromatography with tandem mass spectrometry

The increasing use of antibiotics has caused substantial environmental problems, which are a matter of great concern. The aim of this work was to develop a quick, easy, cheap, effective, rugged, and safe method for 20 antibiotic residues in soil. The developed method is based on extraction with acetonitrile and phosphate buffer, clean up with dispersive solid‐phase extraction adsorbent using primary secondary amine, octadecylsilane, followed by liquid chromatography with tandem mass spectrometry determination. We optimized different extraction methods and the ratio of cleanup adsorbents to achieve good recoveries at seven spiking levels that ranged from 61.4 to 118.9% with a relative standard deviation below 20% (n  = 5). The method quantification limit was in the range of 2–5 μg/kg for most analytes. Good linear regression coefficients greater than 0.990 were obtained. This method was applied for the analysis of real agricultural soil samples, confirming the feasibility of the method.     

Determination of Propylenethiourea,the Main Metabolite of Propineb,in Tomato by HILIC-MS

A quantitative acetonitrile extraction with dispersive solid-phase clean-up and subsequent high performance hydrophilic interaction liquid chromatography-atmospheric pressure electrospray ionization mass spectrometry (HILIC-ESI-MS-MS) analysis is outlined for the determination of propylenethiourea (PTU, 4-methylimidazolidine-2-thione), the main degradation product of propylenebisdithiocarbamate (PBDC). In the present study, the quick, easy, cheap, effective, rugged and safe method (QuEChERS) methodology was adopted for the extraction of PTU from tomato matrix. The synthesis and impurity profiling of a new internal standard compound (4,5-dimethylimidazolidine-2-thione) is also reported, which was used instead of tris(1,3-dichlorisopropyl)phosphate due to poor ionization at elevated acetonitrile levels. The effect of chromatographic parameters on the HILIC separation and MS detection was studied. Coupling of hydrophilic interaction liquid chromatography with mass spectrometric detection was advantageous not only in view of separation and ionization efficiency but also in direct injection of the QuEChERS extract without the need for solvent exchange.     

Application of high‐surface‐area graphitized carbon black with primary secondary amine as an alternative quick,easy, cheap,effective, rugged,and safe cleanup material for pesticide multi‐residue analysis in spinach

A multi‐residue method has been developed and validated to determine 46 pesticides in spinach using liquid chromatography tandem mass spectrometry. The method is based on modified quick, easy, cheap, effective, rugged, and safe sample preparation, where high‐surface‐area graphitized carbon black was used first as sorbent material in the dispersive solid‐phase extraction. The method was compared with the quick, easy, cheap, effective, rugged, and safe method. The morphology, surface area, pore size, and pore volume of the sorbent was determined. The results obtained show that the sorbent consists of high surface area (233 m²/g) and large pore volume (1.5 cm³/g). The calibration curve correlation coefficient (R²) of the method was at least 0.99. The average recoveries ranged from 74 to 116%, and limits of detection and quantification from 0.0001 to 0.002 mg/kg and from 0.0002 to 0.005 mg/kg, respectively. Using the method, the pesticides exhibited low matrix effect (< 20%), except for nicosulfuron (29.86%), methomyl (26.77%), and flufenoxuron (24.65%). The method showed better potential to remove pigments than the quick, easy, cheap, effective, rugged, and safe method. It is demonstrated that the proposed method could be useful alternative for sample preparation of spinach and other matrices in future.     

New analytical method for the determination of musks in personal care products by Quick,Easy, Cheap,Effective, Rugged,and Safe extraction followed by GC–MS

Synthetic musks are organic compounds used as fragrance additives and fixative compounds in a diversity of personal care products. A new method based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction followed by GC–MS for the analysis of 12 musks in personal care products was developed and validated. Some experimental parameters, such as total QuEChERS mass, sample mass/solvent volume ratio, type of extraction solvent, as well as salts and sorbents amount were investigated and optimized. The final method involves the musks extraction using acetonitrile, followed by the addition of anhydrous magnesium sulphate and sodium acetate. The clean‐up step was performed using dispersive SPE with primary and secondary amine and octadecyl–silica sorbents. This extraction procedure is fast (about 10 min) when compared to other traditional approaches. The method was robust for the matrices studied and shows a high precision (%RSD < 15%) and accuracy (average recovery of 85%), allowing the detection of musks in minimum concentrations between 0.01 ng/g (galaxolide) and 15.80 ng/g (musk xylene). The developed method was applied to the analysis of 12 samples, which revealed musks concentrations ranging from 2 ng/g (toothpaste) to 882 340 ng/g (perfumed body lotion).     

Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection

Validation experiments were conducted of a simple, fast, and inexpensive method for the determination of 229 pesticides fortified at 10-100 ng/g in lettuce and orange matrixes. The method is known as the quick, easy, cheap, effective, rugged, and safe (QuEChERS) method for pesticide residues in foods. The procedure involved the extraction of a 15 g sample with 15 mL acetonitrile, followed by a liquid-liquid partitioning step performed by adding 6 g anhydrous MgSO4 plus 1.5 g NaCl. After centrifugation, the extract was decanted into a tube containing 300 mg primary secondary amine (PSA) sorbent plus 1.8 g anhydrous MgSO4, which constituted a cleanup procedure called dispersive solid-phase extraction (dispersive SPE). After a second shaking and centrifugation step, the acetonitrile extract was transferred to autosampler vials for concurrent analysis by gas chromatography/mass spectrometry with an ion trap instrument and liquid chromatography/tandem mass spectrometry with a triple quadrupole instrument using electrospray ionization. Each analytical method was designed to analyze 144 pesticides, with 59 targeted by both instruments. Recoveries for all but 11 of the analytes in at least one of the matrixes were between 70-120% (90-110% for 206 pesticides), and repeatabilities typically <10% were achieved for a wide range of fortified pesticides, including methamidophos, spinosad, imidacloprid, and imazalil. Dispersive SPE with PSA retained carboxylic acids (e.g., daminozide), and <50% recoveries were obtained for asulam, pyridate, dicofol, thiram, and chlorothalonil. Many actual samples and proficiency test samples were analyzed by the method, and the results compared favorably with those from traditional methods.     

Multiresidue method for the determination of 227 pesticides in hot pepper (Capsicum annuum L.) by liquid chromatography with tandem mass spectrometry†

A high‐throughput, rapid, and efficient modified QuEChERS (quick, easy, cheap, effective, rugged, and safe) method with a simple cleanup procedure has been developed for simultaneously determining 227 pesticides in pepper samples by liquid chromatography with tandem mass spectrometry (running time: 10 min). Pesticide residues were extracted/partitioned with an acetonitrile/DisQuE QuEChERS pouch, and the resulting samples were cleaned up with different methods: dispersive solid‐phase extraction with primary secondary amines or multiwalled carbon nanotubes and graphitized carbon solid mini cartridge column. The results indicated that multiwalled carbon nanotubes dispersive sorbents achieved the best recoveries and had less matrix interference. The numbers of pesticides with a recovery in the range of 70–120% were 199 at a spiked level of 40 μg/kg. The correlation coefficients (r²) for 227 pesticides were above 0.99, while the limits of quantitation of pesticides in pepper samples ranged from 0.13 to 13.51 μg/kg (S/N = 10), and the limits of detection ranged from 0.04 to 4.05 μg/kg (S/N = 3). The relative standard deviations of approximately 197 pesticides were below 20% at spiked levels of 40 μg/kg. Based on these results, the proposed method was chosen as the most suitable cleanup procedure for the determination of multiresidue pesticides in pepper samples.     

Fast analysis of 19 anabolic steroids in bovine tissues by high performance liquid chromatography with tandem mass spectrometry

For the detection of 19 steroid hormones in bovine muscle, a fast and sensitive liquid chromatography with electrospray ionization tandem mass spectrometry method was developed using both positive and negative ionization mode. Chromatographic separation on Poroshell 120‐EC C18 column was achieved in less than 10 min using isocratic elution of mobile phase of acetonitrile/methanol/water. The compounds were extracted from muscle tissue using ethyl acetate and quick, easy, cheap, effective, rugged, and safe technique. The purification of the obtained extract was performed by dispersive solid‐phase extraction with sorbents C18, primary secondary amine and magnesium sulphate. The method was validated in accordance with the Commission Decision 2002/657/EC. For all steroids tested good recoveries were obtained (from 51.2 to 121.4%) in the concentration range from decision limits until 5 µg/kg. The values of decision limits and the detection capabilities for individual compounds were in the range 0.10–0.48 and 0.17–0.95 µg/kg, respectively. The method was characterized by satisfactory linearity for most compounds (correlation coefficients  > 0.99) and the reproducibility was lower than 35%. The elaborated procedure has met the criteria for confirmatory methods and is currently used in the official control of hormones.     

Review of the QuEChERS method for the analysis of organic pollutants: Persistent organic pollutants,polycyclic aromatic hydrocarbons,and pharmaceuticals

In multi-residue pesticide analysis, the quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction method has replaced less efficient traditional extraction methods due to its many advantages. In addition to pesticide analysis, this method has been widely used for the detection and analysis of pharmaceuticals, polycyclic aromatic hydrocarbons (PAHs), and several persistent organic pollutants (POPs), including dioxins, polychlorinated biphenyls, perfluoroalkyl substances, and brominated flame retardants in food, biological, and environmental matrices. The analysis of PAHs and POPs is challenging due to the properties of the target compounds and their low concentrations in complex matrices. This review summarizes previously reported the QuEChERS extraction approaches to the analysis of a wide range of analytes. The QuEChERS approaches, which include dispersive solid phase extraction (d-SPE), have generally been combined with either gas chromatography–mass spectrometry (GC–MS) or liquid chromatography–mass spectrometry (LC–MS) analysis. Further on, in recent years, GC and LC-tandem mass spectrometry has been utilized with the QuEChERS extraction due to its high selectivity, sensitivity, and specificity. This enables the extraction methods for target analytes to be modified through the selection of different extraction solvents, salt formulations, and buffers for salting-out partitioning and the selection of different d-SPE and SPE sorbents for the clean-up process. The most significant advantage of this method is that concentration steps are not required. This review aims to provide an up-to-date overview of information regarding the modification of extraction techniques based on target compounds and sample matrices.     

Rapid analysis of organic farming insecticides in soil and produce using ultra-performance liquid chromatography/tandem mass spectrometry

A new method for the analysis of three ecological insecticides, namely azadyrachtin, spinosad (sum of spinosyn A and spinosyn D) and rotenone, in produce and soil samples is presented. Investigated compounds are one of the most significant insecticides authorized for organic farming crop protection in many countries. Extraction of the pesticides from plant and soil matrices was performed by using a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method. The method entailed a single extraction of the investigated compounds with acidified acetonitrile followed by a dispersive solid-phase extraction cleanup step prior to the final determination by reverse-phase ultra-performance liquid chromatography/tandem quadrupole mass spectrometry (UPLC-MS/MS). Validation studies were carried out on cabbage, tomato and soil samples. Recoveries of the spiked samples were in the range between 67% and 108%, depending on the matrix and the spiking level. Relative standard deviations for all matrix–compound combinations did not exceed 12%. The limits of quantification were ≤0.01 mg kg⁻¹ in all cases, except for azadirachtin. The developed method was applied to the analysis of real samples originating from organic farming production.     

Identification of 19 phthalic acid esters in dairy products by gas chromatography with mass spectrometry

A detection method for 19 kinds of phthalic acid ester compounds analyzed by n‐hexane/ether/acetonitrile 1:7:8 v/v/v mixed solvent extraction, quick, easy, cheap, effective, rugged, and safe purification and internal standard method of quantitative gas chromatography with mass spectrometry was established. This method can effectively remove interfering materials, such as lipids, fatty acids, and pigments, from dairy products. The 19 kinds of phthalic acid ester compounds were within a 0.025–0.2 mg/kg range, the recovery rate was 65.2–125.7%, relative standard deviation was 7.9–15.4% (n = 6), and the limit of detection was 0.005–0.02 mg/kg. Concentrations of the 19 kinds of phthalic acid ester compounds ranged between 0.01 and 0.12 mg/kg in ten dairy materials and 20 dairy products. The established method is simple, rapid, accurate, and highly sensitive.     

Residue determination of plant activator benzo‐1,2,3‐thiadiazole‐7‐ carboxylic acid 2‐benzoyloxyethyl ester in water,soil, and vegetable by gas chromatography with tandem mass spectrometry

This study aimed to develop a rapid, specific and sensitive method for the residue determination of benzo‐1,2,3‐thiadiazole‐7‐carboxylic acid 2‐benzoyloxyethyl ester in soil, vegetable, and water by using gas chromatography with tandem mass spectrometry. During the extraction procedure, modified quick, easy, cheap, effective, rugged, and safe method using acetonitrile was compared with classical oscillating extraction using ethyl acetate and acetone, respectively. Before injection, a solid‐phase extraction cartridge of Bond Elut Florisil was used for sample clean‐up. The method was fully validated and showed satisfactory linearity (r² > 0.99) over the range to be assayed (10–1000 ng/mL), with the limits of detection ranging from 0.092–0.229 ng/mL and the limits of quantification ranging from 0.307–0.763 ng/mL. Recovery values at the spiked concentrations of 10, 100 and 1000 ng/g varied from 85.9–109.3%, 81.0–108.2%, 74.2–113.4% for water, soil and vegetable, respectively, with the maximum relative standard deviations of 12.2%. Results indicated that the established modified quick, easy, cheap, effective, rugged, and safe method coupled to gas chromatography with tandem mass spectrometry was promising for the residue monitoring of benzo‐1,2,3‐thiadiazole‐7‐carboxylic acid 2‐benzoyloxyethyl ester in the environment and vegetable products.     

Determination of diflubenzuron and chlorbenzuron in fruits by combining acetonitrile‐based extraction with dispersive liquid–liquid microextraction followed by high‐performance liquid chromatography

In this study, a simple and low‐organic‐solvent‐consuming method combining an acetonitrile‐partitioning extraction procedure followed by “quick, easy, cheap, effective, rugged and safe” cleanup with ionic‐liquid‐based dispersive liquid–liquid microextraction and high‐performance liquid chromatography with diode array detection was developed for the determination of diflubenzuron and chlorbenzuron in grapes and pears. Ionic‐liquid‐based dispersive liquid–liquid microextraction was performed using the ionic liquid 1‐hexyl‐3‐methylimidazolium hexafluorophosphate as the extractive solvent and acetonitrile extract as the dispersive solvent. The main factors influencing the efficiency of the dispersive liquid–liquid microextraction were evaluated, including the extractive solvent type and volume and the dispersive solvent volume. The validation parameters indicated the suitability of the method for routine analyses of benzoylurea insecticides in a large number of samples. The relative recoveries at three spiked levels ranged between 98.6 and 109.3% with relative standard deviations of less than 5.2%. The limit of detection was 0.005 mg/kg for the two insecticides. The proposed method was successfully used for the rapid determination of diflubenzuron and chlorbenzuron residues in real fruit samples.     

Sample preparation for planar chromatography

High-performance thin-layer chromatography has favorable properties for high-throughput separations with a high matrix tolerance. Sample preparation, however, is sometimes required to control specific matrix interferences and to enhance the detectability of target compounds. Trends in contemporary applications have shifted from absorbance and fluorescence detection to methods employing bioassays and mass spectrometry. Traditional methods (shake-flask, heat at reflux, Soxhlet, and hydrodistillation) are being challenged by automated instrumental approaches (ultrasound-assisted and microwave-assisted solvent extraction, pressurized liquid extraction, and supercritical fluid extraction) and the quick, easy cheap, efficient, rugged, and safe extraction method for faster and streamlined sample processing. Liquid-liquid extraction remains the most widely used approach for sample clean-up with increasing competition from solid-phase extraction. On-layer sample, clean-up by planar solid-phase extraction is increasingly used for complex samples and in combination with heart-cut multimodal systems. The automated spray-on sample applicator, the elution head interface, biological detection of target and non-target compounds, and straightforward mass spectrometric detection are highlighted as the main factors directing current interest toward faster and simpler sample workflows, analysis of more complex samples, and the determination of minor contaminants requiring high concentration factors.     

Simultaneous determination of pinoxaden,cloquintocet-mexyl,clodinafop-propargyl ester and its major metabolite in barley products and soil using QuEChERS modified with multi-walled carbon nanotubes coupled with LC–MS/MS

Herein, a modified quick, easy, cheap, effective, rugged, and safe (QuEChERS) method with multi-walled carbon nanotube (MWCNT) as a dispersive solid-phase extraction was developed for simultaneous determination of pinoxaden (PXD), cloquintocet-mexyl (CLM), clodinafop-propargyl ester (CPE) and its major metabolite (clodinafop, CP) in barley grass powder, barley grain, and soil using liquid chromatography–tandem mass spectrometry (LC–MS/MS). We found that MWCNT as an absorbent could improve the recoveries of the tested analytes, particularly CP, in complex matrices. Under the optimum conditions, the established MWCNT-modified QuEChERS coupled with LC–MS/MS method exhibited excellent linearity (R²) of ≥0.9912, low limits of detection (LODs) and quantification (LOQs) of 0.02–0.07 and 0.29–1.26 μg kg⁻¹, and acceptable recoveries of 80–130% with intra- and inter-day relative standard deviations (RSDs) < 10.5%. No strong matrix effect (ME) has been observed on the respective samples. The method was successfully applied to monitor the tested analytes in the representative field incurred samples. Conclusively, the proposed method is sensitive and reliable and could be used to monitor the residues of PDX, CLM, CPE, and CP in complicated agro-products and soil matrices.     

Simultaneous determination of pyrametostrobin and its two metabolites in cucumber and soil using a quick,easy, cheap,effective, rugged,and safe method with HPLC–MS/MS

An easy, effective and sensitive analytical method for the simultaneous determination of a novel fungicide pyrametostrobin and its two metabolites pyrametostrobin‐M1 and pyrametostrobin‐M2 in cucumber and soil was developed using a quick, easy, cheap, effective, rugged, and safe method with high‐performance liquid chromatography and tandem mass spectrometry. The extraction solvent was acetonitrile, and cleanup sorbents were primary secondary amine and graphitized carbon black for cucumber samples and primary secondary amine for soil samples. The three target compounds were successfully separated between 3.2 and 3.9 min using a Waters CORTECS™ C₁₈ column connected to an electrospray ionization source. All the matrix‐matched samples at three fortified levels (10, 100 and 1000  μg/kg) provided satisfactory recoveries in the range of 78.8–93.8% with relative standard deviations below 6.9%. The limits of quantitation for the three compounds were below 0.183 μg/kg. The proposed method was validated by analyzing real samples.     

Development and evaluation of microwave‐assisted and ultrasound‐assisted methods based on a quick,easy, cheap,effective, rugged,and safe sample preparation approach for the determination of bisphenol analogues in serum and sediments

Microwave‐ and ultrasound‐assisted methods based on a quick, easy, cheap, effective, rugged, and safe sample preparation approach followed by high‐performance liquid chromatography with tandem mass spectrometry were developed for the simultaneous determination of eight bisphenol analogues in serum and sediment. The developed methods provided satisfactory extraction efficiency for the energy provided by microwaves and ultrasound. Compositions of commercial sorbents (primary secondary amine, MgSO₄, octadecyl‐modified silica, and graphitized carbon black) were evaluated. The ultrasound‐assisted method was suited for serum using primary secondary amine, MgSO₄, and octadecyl‐modified silica as sorbents and a mixture of hexane and ethyl acetate as extraction solvent. The microwave‐assisted method worked better for sediment with tetrahydrofuran and methanol as solvents and primary secondary amine, MgSO₄, octadecyl‐modified silica, and graphitized carbon black as sorbents. Other experimental parameters, such as extraction temperature and time, were also optimized. The inter‐ and intraday relative standard deviations ranged from 2.7 to 5.5%. The limits of detection were between 0.1 and 1.0 ng/mL for serum and between 0.1 and 0.5 ng/g dry weight for sediment. The proposed methods were successfully applied to seven sediment and 20 human serum samples. The results showed that the developed methods were practical for the analysis and biomonitoring of bisphenols in sera and sediment.     

Quantification of artesunate and its metabolite,dihydroartemisinin, in animal products using liquid chromatography–tandem mass spectrometry

An analytical approach using a modified quick, easy, cheap, effective, rugged, and safe extraction method followed by liquid chromatography with electrospray ionization tandem mass spectrometry was developed herein for the determination of artesunate and its metabolite, dihydroarteminsinin in porcine muscle, egg, eel, flatfish, and shrimp. 10% trichloroacetic acid in acetonitrile mixed with ethyl acetate was used as an extraction solvent. To obtain a good separation, a Phenomenex Kinetex reversed‐phase analytical column was selected with mobile phase consisting of distilled water (A) and acetonitrile (B), both containing 0.05% formic acid. Good linearity was achieved using matrix‐matched calibrations constructed from six concentrations (5–50 μg/kg) with determinant coefficients ≥0.9918. Recoveries estimated from three spiking concentrations (5, 10, and 20 μg/kg) ranged between 71.3 and 104.7% in all matrixes with relative standard deviations ≤8.3%. A variety of samples purchased from markets in Seoul were tested following the protocol described herein. The artesunate and dihydroarteminsinin were not detected in any matrix. The methodology proposed could be used for routine determination of artesunate and its metabolite, dihydroartemisinin in various animal products having variable percentages of fat and protein.     

改进的QuEChERS方法结合液相色谱-串联质谱法测定腐竹和豆干中的二甲基黄和二乙基黄

建立了基于改进的QuEChERS方法结合液相色谱-串联质谱测定腐竹和豆干中二甲基黄和二乙基黄的方法。在2.0 g腐竹和豆干样品中加入5 mL水浸泡,然后加入10 mL乙腈提取,加入1.0 g NaCl、2.0 g无水硫酸镁进行液液分离;取1 mL提取液经50 mg N-丙基二乙胺分散固相萃取净化,经液相色谱分离、质谱测定,外标法定量。二甲基黄在添加水平为0.3、1和10 μg/kg时,方法的回收率为73.5%~84.5%;二乙基黄在添加水平为0.1、1和10 μg/kg时,方法的回收率为70.5%~81.2%;方法的相对标准偏差小于11%。二甲基黄的检出限和定量限分别为0.1 μg/kg和0.3 μg/kg,二乙基黄的检出限和定量限分别为0.05 μg/kg和0.1 μg/kg。该方法可以用于腐竹、豆干中二甲基黄和二乙基黄的快速筛查和定量分析。