Reversed migration micellar electrokinetic chromatography with off-line and on-line concentration analysis of phenylurea herbicides

Three environmentally important phenylurea herbicides (monuron, isoproturon, diuron) were separated in reversed migration micellar electrokinetic chromatography (RM-MEKC) using 50 mM sodium dodecyl sulfate, 50 mM phosphoric acid, and 15 mM gamma-cyclodextrin. Three on-line concentration techniques are then evaluated to increase the detection sensitivity of the RM-MEKC system. Stacking with reverse migrating micelles (SRMM, water as the sample solvent) provided the best results among the focusing techniques studied. Using a z-shaped detection cell, more than 500-fold increase in peak height is obtained. As a sample preparation and off-line concentration method, solid-phase extraction (SPE) that further improved detection sensitivity was used in the analysis of spiked tap and pond water. For example, 1 parts per billion of each herbicide spiked in tap or pond water was detected by MEKC after SPE and SRMM.     

Investigation of preconcentration strategies for the trace analysis of multi-residue pesticides in real samples by capillary electrophoresis

In this work, on-line preconcentration strategies were investigated for the multi-residue analysis of pesticides in drinking water and vegetables using micellar electrokinetic chromatography. Among the on-line strategies, sweeping and stacking with reverse migration of micelles (SRMM), with and without the insertion of a plug of water before sample injection, were contrasted. A new version of SRMM was also introduced. The modification consisted of momentarily applying a positive voltage at the inlet vial right after sample has been injected, increasing the efficiency by which the analytes are captured. Nine pesticides from different classes, carbendazim (benzimidazole), simazine, atrazine, propazine and ametryn (triazine), diuron and linuron (urea), carbaryl and propoxur (carbamate), were baseline separated in less than 6 min with a electrolyte composed of 20 mmol l(-1) phosphate buffer at pH 2.5, containing 25 mmol l(-1) sodium dodecyl sulfate and 10% methanol. Limits of detection (LODs) in the order of 2-46 microg l(-1) for the pesticides under investigation were obtained solely using the on-line strategies. Enrichment factors of 3-18-fold were obtained. These factors were computed as the improvement of the concentration LODs with respect to the reference condition (injection of 10 s at 2.5 kPa pressure). The proposed methodologies were applied to the analysis of pesticides in complex matrices such as carrot extracts where the detection of 2.5 microg l(-1) was illustrated. By combining off-line solid-phase extraction and the proposed on-line strategies, the detection of pesticides in drinking water at the 0.1 microg l(-1) level was conceived.     

Different sample stacking strategies to analyse some nonsteroidal anti-inflammatory drugs by micellar electrokinetic capillary chromatography in mineral waters

Three on-column preconcentration techniques were compared to analyse a group of nonsteroidal anti-inflammatory drugs (NSAIDs) using micellar electrokinetic capillary chromatography (MEKC) under pH-suppressed electroosmotic flow (EOF) in water samples. The analysed drugs were ibuprofen, fenoprofen, naproxen, ketoprofen, and diclofenac sodium. The micellar background electrolyte (BGE) solution was formed by 75 mM sodium dodecyl sulfate (SDS), 40% (v/v) acetonitrile, and 25 mM sodium phosphate at pH 2.5. When this BGE solution was used the applied voltage was reversed, -10 kV, and the drugs were separated within 20 min. The on-column preconcentration modes, characterised all of them for the sample matrix removal out of the capillary by itself under a reverse potential at the same time as the EOF was reduced, were stacking with reverse migrating micelles (SRMM), stacking with reverse migrating micelles-anion selective exhaustive injection (SRMM-ASEI), and field-enhanced sample injection with reverse migrating micelles (FESI-RMM). The sensitivity was improved up to 154-, 263-, and 63-fold, respectively when it was calculated through the peaks height. The optimised methods were validated with spiked mineral water by combining off-line solid-phase extraction (SPE) and the proposed on-line sample stacking strategies. The detection limits (LODs) of NSAIDs in mineral water were at ng/L levels.     

Determination of pesticides in wine using micellar electrokinetic chromatography with UV detection and sample stacking

In this work, the analysis of a group of four fungicides (pyrimethanil, nuarimol, procymidone and cyprodinil) and one insecticide (pirimicarb) by micellar electrokinetic chromatography (MEKC) with UV detection using the on-line preconcentration strategy called reversed electrode polarity stacking mode (REPSM) is proposed. After optimisation, an adequate separation electrolyte for the separation and stacking of these pesticides was obtained which consisted of 100 mM borate, 60 mM sodium dodecyl sulphate (SDS), at pH 9.0 and 2% 2-propanol. The use of this running buffer together with the REPSM preconcentration method provided limits of detection (LODs) between 38.3 and 241 microg/L. In order to apply the developed methodology for the analysis of these pesticides in wine samples, several off-line preconcentration strategies (mainly, solid-phase extraction, SPE, and solid-phase microextraction, SPME) were tested. Although the use of a SPE procedure, optimized in this work for water samples, using Oasis HLB cartridges, provided mean recovery values between 79 and 100% for spiked water samples, it could not be applied to the extraction of these pesticides from wine samples due to high interference from the sample matrix. However, the use of a SPME procedure using polydimethylsiloxane/divynilbenzene (PDMS/DVB) fibers allowed the selective extraction of four of the five pesticides which could be perfectly determined. The final combination of the off-line SPME and on-line REPSM preconcentration strategies allowed obtaining LODs between 17.6 and 32.3 microg/L.     

Comparison of two sample preconcentration strategies for the sensitivity enhancement of flavonoids found in Chinese herbal medicine in micellar electrokinetic chromatography with UV detection

Two on-column preconcentration techniques named stacking with reverse migrating micelles (SRMM) and anion selective electrokinetic injection and a water plug-sweeping with reverse migrating micelles (ASIW-sweep-RMM) were used and compared for concentration and separation of flavonoids in Chinese herbs using reverse migration micellar electrokinetic chromatography (RM-MEKC). The optimal background electrolyte (BGE) used for separation and preconcentration was a solution composed of 20mM phosphoric acid (H(3)PO(4))-100mM sodium dodecyl sulfate (SDS)-20% (v/v) acetonitrile (ACN) buffer (pH 2.0), the applied voltage was -15kV. To achieve reasonable results of the two techniques, the conditions which affected preconcentration were examined. A comparison of used techniques with normal hydrodynamic injection (5s), concerning enhancement factors and limits of detection (LODs) was presented. Under the optimum stacking conditions, about 27-37- and 45-194-fold improvement in the detection sensitivity was obtained for SRMM and ASIW-sweep-RMM, respectively, compared to usual hydrodynamic sample injection (5s). The LODs (S/N=3) for SRMM and ASIW-sweep-RMM in terms of peak height, can reach down to 1.15 x 10(-2) microg/ml for hesperetin and 2.4 x 10(-3) microg/ml for nobiletin, respectively. Finally, the amounts of the six flavonoids in extract of Fructus aurantii Immaturus were successfully determined using ASIW-sweep-RMM. The six analytes were baseline separated with sample matrix under the optimum ASIW-sweep-RMM conditions and the experimental results showed that preconcentration was well achieved after the dilution of sample solutions.     

Different sample stacking strategies for the determination of ertapenem and its impurities by micellar electrokinetic chromatography in pharmaceutical formulation

Ertapenem, a Group 1 carbapenem, is most recently introduced into the market. It is a beta-lactam antibiotic that possesses a broad antibacterial spectrum including common community-acquired Gram-positive and Gram-negative aerobic and anaerobic pathogens, but low activity against some nosocomial pathogens such as Pseudomonas aeruginosa, Acinetobacter spp., enterococci and methicillin-resistant staphylococci. The elaborated method of micellar electrokinetic chromatography (MEKC) of ertapenem separation from its impurities was successfully performed using normal stacking mode (NSM) and stacking with reverse migrating micelles (SRMM), followed by UV absorption detection at 214 nm. The best results were obtained with 60mM sodium dihydrogen phosphate and 20mM boric acid buffer pH 6.0, as background electrolyte. Uncoated fused-silica capillary and neutral-coated capillary with normal and reverse polarity, and voltage values of +18 and -12 kV, respectively, were used throughout the investigation. Sodium dodecyl sulfate was employed as the pseudostationary phase. A comparison of applied techniques, including sensitivity enhancement factors and limits of detection (LOD), is presented. The optimized method was validated in terms of linearity, accuracy and precision. Comparable LOD was obtained using both stacking methods (0.3 microg/mL) but better efficiency of ertapenem peak was obtained using NSM. Under the optimum stacking conditions, about 183-4.75-fold and 1289-4.07-fold improvements in peak areas were obtained for NSM and SRMM, respectively, compared to the usual hydrodynamic sample injection (10s). The reproducibility, expressed by relative standard deviations (RSD) of the migration times, for NSM was about 0.96-1.25 and for SRMM was 0.32-0.45. The RSD of corrected peak areas, for NSM was about 1.07-8.14 and for SRMM was 0.74-8.12. The difference in separation time between the two techniques was not obvious. Satisfactory separation was possible after less than 11min of electrophoresis. The evaluated MEKC method was applied in the analysis of medicinal product containing ertapenem: Invanz-ertapenem for injection.     

Determination of pesticides in drinking water by micellar electrokinetic capillary chromatography

A new analytical procedure using a two-step sample preconcentration (solid-phase extraction (SPE) and field-amplified sample stacking) prior to separation by micellar electrokinetic capillary chromatography was developed for the determination of 14 pesticides such as aldicarb, carbofuran, isoproturon, chlorotoluron, metolachlor, mecoprop, dichlorprop, MCPA, 2,4-D, methoxychlor, TDE, DDT, dieldrin, and DDE in drinking water. Good recoveries of pesticides were obtained using SPE with sample pH adjusted to 2-3. Field-amplified sample stacking was found to give enrichment factors up to 30-fold preconcentration of various pesticides under reversed polarity at -2 kV for 50 s. The optimized background electrolyte (BGE) consisted of 50 mM sodium dodecyl sulfate (SDS), 10 mM borate buffer, 15 mM beta-cyclodextrin (beta-CD), and 22% acetonitrile at pH 9.6, running was under 25 kV and detection at 202 nm. Good linearity was obtained for all pesticides with detection limits down to 0.04-0.46 ng/mL and a working range of 0.1-40 ng/mL. The repeatabilities of migration time and peak area were satisfactory with relative standard deviations (RSDs) between 0.66 and 13.6% and 4.1 and 28%, respectively. All pesticides except dieldrin were found to be detected at concentrations at least tenfold lower than the World Health Organization (WHO) guideline values. The analytical procedure developed offers an economic method for fast screening of multiple pesticide residues in drinking water for health protection. It had been applied to determine carbofuran and MCPA in agricultural run-off water samples, giving satisfactory repeatabilities of 10 and 12%, respectively, with n=5 for the determination of pesticides in contaminated water samples.     

肌肽类生物活性肽的毛细管电泳在线富集技术

建立了毛细管区带电泳(CZE)在线富集3种肌肽类活性肽(肌肽、鹅肌肽和高肌肽)的两种简便有效的方法。一种是大体积进样反向压力排除基体富集（LVSRP）技术,即通过流体动力学进样,在不改变电源极性的条件下,利用反向压力排除样品基体,电堆积富集后进行CZE分离;另一种是大体积进样电渗流排除基体富集（LVSEP）技术,即通过流体动力学进样,于运行缓冲液中加入溴化十六烷基三甲基铵(CTAB)动态修饰毛细管表面,通过电渗流排除样品基体,改变电源极性后进行CZE分离。与常规CZE相比,LVSRP技术和LVSEP技术使检测灵敏度提高了40~60倍。对影响两种富集过程的一些因素进行了研究,在最优富集条件下考察本方法的线性范围为0.080~5.0 μmol/L。对3种生物活性肽的检测限(S/N=3)分别为LVSRP 41~58 nmol/L,LVSEP 35~43 nmol/L。     

Determination of herbicides in mineral and stagnant waters at ng/L levels using capillary electrophoresis and UV detection combined with solid-phase extraction and sample stacking

In this work, the combined use of solid-phase extraction (SPE) and on-line preconcentration strategies as normal stacking mode (NSM) and stacking with matrix removal (SWMR) for the ultrasensitive and simultaneous capillary electrophoresis-ultraviolet analysis (CE-UV) of five triazolopyrimidine sulfonanilide pesticides (i.e., diclosulam, cloransulam-methyl, flumetsulam, metosulam and florasulam) in different types of water is investigated. An adequate separation electrolyte for the separation and stacking of these pesticides was obtained, considering also its compatibility with MS detection, which consisted of 24 mM formic acid and 16 mM ammonium carbonate at pH 6.4. It was observed that the use of this running buffer together with the SWMR preconcentration method provided the best results in terms of sensitivity (between 6.54 and 11.9 microg/L) and peak efficiency (up to 550000 theoretical plates per meter, NTP/m). When this on-line preconcentration procedure was combined with an off-line sample preconcentration step as SPE using C18 cartridges, the selected herbicides could be detected in the ng/L range. The optimized SPE-SWMR-CE-UV method was applied to the determination of the selected group of pesticides in spiked and non-spiked mineral and stagnant waters. Recoveries ranged between 55 and 110% and limits of detection between 131 and 342 ng/L. This work shows the great possibilities of the combined use of SPE-SWMR-CE-UV to overcome the sensitivity problems usually linked to CE analysis.     

Off-Line Concentration of Bisphenol A and Three Alkylphenols by SPE then On-Line Concentration and Rapid Separation by Reverse-Migration Micellar Electrokinetic Chromatography

A method for separation of four environmentally important compounds (three alkylphenols and bisphenol A) by cyclodextrin-modified reverse-migration micellar electrokinetic chromatography (CD-RM-MEKC) has been optimized. On-line concentration, stacking using reverse-migrating micelles and a water plug (SRW), was used to improve the limit of detection. Two main factors affecting the efficiency of enhancement by SRW, injection sample length and water-plug length, are discussed in detail. Compared with the normal 2-s injection, more than 121-fold enhancement of peak area and more than 71-fold enhancement of peak height were achieved with 120-s sample injection after 120-s water-plug injection. With this optimized separation method and SRW technology, limits of detection were found to be 0.089, 0.030, 0.0091, and 0.033 mg L^–1 for 4-nonylphenol, 4-tert-octylphenol, bisphenol A, and 4-tert-butylphenol, respectively. Calibration plots (R² 0.9968) and relative standard deviations (RSD, %) of corrected peak areas and migration time were also satisfactory. Combined with off-line concentration by solid-phase extraction (SPE) this method might be used to determine these contaminants at ppb levels in groundwater samples.     

Highly-sensitive micellar electrokinetic chromatographic analysis of dioxin-related compounds using on-line concentration.

An application study of an on-line concentration technique of neutral analytes for micellar electrokinetic chromatography (MEKC) was carried out in environmental analysis to enhance the UV detection sensitivity. Several dioxins and related compounds, such as dibenzofuran, dibenzo-p-dioxin, 2,3- and 2,7-dichlorodibenzo-p-dioxins, and 2,3,7-trichlorodibenzo-p-dioxin, were used as test solutes. For a highly sensitive separation and detection, cyclodextrin-modified MEKC (CD-MEKC) under acidic conditions was employed as a separation mode and stacking using reverse migrating micelles and a water plug (SRW) as an on-line concentration technique. Almost a 200-fold gain in detection sensitivity was obtained for the model compounds in SRW-CD-MEKC compared to that in normal CD-MEKC without on-line concentration and the limit of detection was found to be around 0.1 ppm for each solute.     

On-line stacking techniques for the nonaqueous capillary electrophoretic determination of acrylamide in processed food

In the present study, field amplified sample stacking (FASS) techniques in the nonaqueous capillary electrophoresis method (NACE) were introduced for the on-line concentration of the acrylamide to improve acrylamide detection at 210 nm by diode-array detection. Acetonitrile (ACN) as a nonaqueous solvent permits acrylamide to be protonated through the change of its acid-base chemistry, allowing capillary electrophoretic separation of this compound. Choosing 30 mmol L(-1) HClO(4), 20 mmol L(-1) NaClO(4), 218 mmol L(-1) CH(3)COOH in ACN as the separation electrolyte and employing sample stacking methods, the LOD value of acrylamide was decreased to 2.6 ng mL(-1) with electrokinetic injection and 4.4 ng mL(-1) with hydrodynamic injection. Optimized stacking conditions were applied to the determination of acrylamide in several foodstuffs. The method is simple, rapid, inexpensive, and widely applicable for the determination of acrylamide in food samples.     

Analysis of cytokinin nucleotides in coconut (Cocos nucifera L.) water using capillary zone electrophoresis-tandem mass spectrometry after solid-phase extraction

A method based on solid-phase extraction (SPE) and capillary zone electrophoresis-tandem mass spectrometry (CZE-MS/MS) is described for the separation and determination of six cytokinin nucleotides in coconut water. The best CZE separation for the six cytokinin nucleotide standards was achieved using a 25 mM ammonium formate/formic acid buffer (pH 3.8) and 2% (v/v) methanol with an applied gradient separation voltage (25 kV for 32 min, and then a linear gradient to 30 kV in 5 min, finally 30 kV to the end of separation) in less than 60 min. MS/MS with multiple reaction monitoring (MRM) detection was carried out to obtain sufficient selectivity and sensitivity for the cytokinin nucleotides. The combined use of on-line sample stacking and CZE-MS/MS achieved limits of detection (LODs) in the range of 0.06-0.19 microM for the six cytokinin nucleotides at a signal-to-noise ratio of 3. Furthermore, a novel dual-step SPE procedure was developed for the pre-concentration and purification of cytokinin nucleotides using Oasis HLB and Oasis MAX cartridges. The recoveries of the cytokinin nucleotides after the dual-step SPE were in the range of 44-71%. The combination of off-line SPE, on-line sample stacking and CZE-MS/MS approach was successfully applied to screen for endogenous cytokinin nucleotides present in coconut water sample. trans-Zeatin riboside-5'-monophosphate (ZMP) was detected and quantified in coconut water by CZE-MS/MS after SPE and on-line sample stacking.     

Determination of regularly distributed plant protectants in raw and drinking waters, using a multiresidue method with cyclodextrin-modified micellar electrokinetic chromatography

Eighteen plant protectant compounds were separated and determined by cyclodextrin-modified micellar electrokinetic chromatography (MEKC) in a multiclass/multiresidue method. The pesticides included are those dispersed in the greatest amounts today over agricultural acreage, and they represent 8 different classes of compounds (azoles, benzoic acids, chloroacetanilides, phenoxy acids, phenylureas, sulfonylureas, thiocarbamates, and triazines) covering a wide range of chemical reactivities and physicochemical properties. A 500 mL sample of tap water is preconcentrated by solid-phase extraction (SPE) with 300 mg combined polystyrene-divinylbenzene and methacrylate macroporous resins. Trapped analytes are eluted collectively with diethyl ether. Concentration and solvent change yield 250 microL of an acetone "concentrate," which is further worked up and concentrated 1:10 to produce the MEKC injection solution containing 10 mmol/L sodium dodecyl sulfate (SDS) surfactant. For MEKC, 2 phosphate/SDS buffer systems were designed, each allowing complete separation of all pesticides in a single run. Sensitivity was enhanced by a self-etched bubble cell and an injection procedure which employs stacking at reversed polarity. The ability of MEKC to determine plant protectants in raw and drinking waters at the 0.1 microgram/L level, as demanded by the guidelines of the European Union, was demonstrated with spiked tap waters. Recoveries were between 75 and 110%, and limits of quantification, evaluated as method detection limits according to guidelines of the U.S. Environmental Protection Agency, ranged between 0.03 and 0.10 microgram/L. The precisions of the relative migration times were all below 0.5%.     

Determination of nine emerging pesticides at trace level in aqueous samples using fully automated on-line solid phase extraction coupled with liquid chromatography-mass spectrometry

On-line solid phase extraction (SPE) coupled to liquid chromatography-mass spectrometry (LC-MS) offers an easy and fast strategy to analyze the organic contaminants in environmental samples with high sensitivity and selectivity. This paper described an in-house designed on-line SPE system and an on-line SPE-LC-MS method for the determination of pesticides at trace levels in water samples. The system was assembled from an eight-position valve, a piston pump, a six-port valve and a C18 SPE column, and significantly reduced analysis time by achieving full automation. Moreover, the use of a large enrichment volume (50?mL) significantly enhanced method sensitivity. Using this on-line SPE system, an on-line SPE-LC-MS method was developed for the determination of nine pesticides at trace levels in lake water and seawater sample. Under optimized conditions, method detection limits (MDLs) were 1.00–10.0?ng?L^?1.     

MEKC combined with SPE and sample stacking for multiple analysis of pesticides in water samples at the ng/L level

In this work, a new multiresidue analytical method based on MEKC with UV detection combined with SPE as off-line preconcentration strategy, and reversed-electrode polarity stacking mode (REPSM) as on-line stacking procedure, has been developed for the monitoring of 12 pesticides (carbendazim, pirimicarb, metalaxyl, pyrimethanil, procymidone, nuarimol, azoxystrobin, tebufenozide, fenarimol, benalaxyl, penconazole, and tetradifon) that are currently being used in the Canary Islands (Spain). The optimized MEKC buffer, consisting of 100 mM sodium tetraborate and 30 mM SDS at pH 8.5 with 6% v/v 1-propanol, provided baseline resolution of the 12 pesticides in less than 20 min. The developed method was applied to the analysis of mineral, stagnant, and tap water samples. The proposed SPE-REPSM-MEKC-UV method showed high extraction efficiencies with detection limits (LODs) at the low ng/L level providing LOD values down to 64 ng/L for these real samples.     

Chemometric modeling of neurotransmitter amino acid separation in normal and reversed migration micellar electrokinetic chromatography

A chemometric experimental design has been applied for the optimization of neurotransmitter amino acid separation in capillary electrophoresis. The optimizations were carried out for normal micellar electrokinetic chromatography (N-MEKC) and reversed migration micellar electrokinetic chromatography (RM-MEKC). In order to optimize three separation factors and study the interaction between factors, a response function was optimized via searching its optimum (minimum/maximum). For this purpose a central composite design with multivariate linear regression (MLR) analysis was utilized. Modeling with good regression coefficients from the MLR adequately described the interaction of factors such as background electrolyte and sodium dodecylsulfate concentrations which had a large impact on selectivity and migration behaviors. Similar optimal conditions regarding resolution and number of theoretical plates but different retention behaviors as a function of background electrolyte and micellar concentrations were observed for N-MEKC and RM-MEKC. Improved overall performance from the RM-MEKC separation of five neurotransmitter acids, superior to N-MEKC, is demonstrated in terms of repeatability, peak symmetry, sensitivity, and in particular, impurity determination in an overloaded separation system.     

Pesticide analysis by micellar electrokinetic capillary chromatography

On-capillary sample concentration using sample stacking for the improvement of detection limits for various pesticides separated by micellar electrokinetic capillary chromatography was examined. The dependence of the stacking on different parameters was investigated. An approximately 30-fold preconcentration was achieved by applying sample stacking. Employing a two-step enrichment process (solid-phase extraction combined with sample stacking), detection limits were improved and the sample volume for SPE was reduced. In addition, the total time for the analysis was considerably reduced. Detection limits were between 0.01 and 0.1 ng/ml under these enrichment conditions.     

在线固相萃取/液相色谱-线性离子阱质谱法同时检测生物样品中18种氨基甲酸酯类农药

建立了同时测定全血、尿液和肝组织等生物样品中18种氨基甲酸酯类农药的在线固相萃取/液相色谱-线性离子阱质谱(On-line SPE/LC-LIT/MS)分析方法。样品经乙腈处理,稀释和离心后直接进样。经Waters OasisHLB在线SPE柱富集纯化,以BETASIL C18柱为分析柱,甲醇-水(均含0.1%甲酸)为流动相进行梯度洗脱;使用电喷雾电离(ESI)正离子模式测定,扫描方式为选择反应监测(SRM)和连续反应监测(CRM)。18种农药在考察的质量浓度范围内线性关系良好(权重因子1/X),相关系数为0.994 3~0.999 4;在全血和尿液中的检出限为0.1~5 ng/m L,在肝组织中的检出限为0.1~5 ng/g;3个加标水平的回收率为90.2%~114.5%,相对标准偏差(n=4)为0.5%~7.5%。该方法简单准确,灵敏度高,能够满足生物样品中18种氨基甲酸酯类农药的快速分析要求。     

Determination of Riboflavin in Cereal Grains by Capillary Electrophoresis with Laser-Induced Fluorescence Detection with On-Line Concentration

A very simple, sensitive, and reliable method for the routine determination of riboflavin in cereal grains by capillary electrophoresis with laser-induced fluorescence detection (CE-LIF) was established. Two on-line concentration techniques, namely, stacking in reverse migrating micelles (SRMM) and sweeping, were examined to enhance the detection signal. The optimum separation buffer consisted of 20 mM phosphoric acid and 140 mM sodium dodecyl sulfate (SDS), and a hydrodynamic injection of 30 s at 0.5 psi was confirmed for the introduction of a sample. In addition, it was found that salt in sample matrix influenced the performance of SRMM, showing the standard addition method was required for the quantitative analysis. The linearity of the method was good with a range of 0.5–500 ng/mL (r = 0.9990). The limit of detection (LOD) was 0.29 ng/mL at a signal-to-noise ratio of 3. This procedure presented was successfully applied to determine riboflavin in 18 samples of 9 types of cereal grains. The recovery rates varied from 94% to 98%, and the relative standard deviation (RSDs) was less than 4.1%.