Preparation and examination of monolithic in-needle extraction (MINE) device for the direct analysis of liquid samples

Combination of extraction and chromatographic techniques opens NEW possibilities in sample preparation area. Macroporous poly(styrene-divinylbenzene) (PS-DVB) monoliths were prepared by in situ polymerization in stainless steel needles. The surface of stainless steel needle was modified earlier by the silane coupling agent. Monolithic materials located inside needles were used as the in-needle extraction device. Scanning electron microscope (SEM) images were obtained for nine monoliths. Spectra of prepared materials were also performed with the use of two techniques: Attenuated Total Reflectance (ATR) and Fourier Transform Infrared Spectroscopy (FTIR). The new monolithic in-needle extraction (MINE) devices were used in the preparation of a series of test water samples for chromatographic analysis. The extraction of phenolic compounds from water samples was carried out by pumping liquid samples through the MINE device. Obtained results indicate a high efficiency of in-needle extraction systems based on monolithic materials. Breakthrough volume and the sorption efficiency of prepared monolithic in-needle extraction devices were determined experimentally. The achieved recovery was close to 90%, and determined LOQ values varied between 0.4 and 6 μg.     

Simple and sensitive monitoring of sulfonamide veterinary residues in milk by stir bar sorptive extraction based on monolithic material and high performance liquid chromatography analysis

A simple, rapid, and sensitive method for the quantitative monitoring of five sulfonamide antibacterial residues (SAs) in milk was developed by stir bar sorptive extraction (SBSE) coupling to high performance liquid chromatography with diode array detection. The analytes were concentrated by SBSE based on poly (vinylimidazole–divinylbenzene) monolithic material as coating. The extraction procedure was very simple, milk was diluted with water then directly sorptive extraction without elimination of fats and protein in samples was required. To achieve optimum extraction performance for SAs, several parameters, including extraction and desorption time, desorption solvent, ionic strength and pH value of sample matrix were investigated. Under the optimized experimental conditions, low detection limits (S/N = 3) quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 1.30–7.90 ng/mL and 4.29–26.3 ng/mL from spiked milk, respectively. Good linearities were obtained for SAs with the correlation coefficients (R²) above 0.996. Finally, the proposed method was successfully applied to the determination of SAs compounds in different milk samples and satisfied recoveries of spiked target compounds in real samples were obtained.     

Sensitive determination of strongly polar aromatic amines in water samples by stir bar sorptive extraction based on poly(vinylimidazole-divinylbenzene) monolithic material and liquid chromatographic analysis

A simple and sensitive method for the determination of polar aromatic amines (PAAs) was developed using stir bar sorptive extraction (SBSE) coupling to high-performance liquid chromatography. A hydrophilic poly(vinylimidazole-divinylbenzene) (VIDB) monolithic material was prepared and acted as SBSE coating. The influences of polymerization conditions for VIDB on the extraction efficiency were investigated using aniline and 2,4-dinitroaniline as detected solutes. To achieve optimum extraction performance for PAAs, several parameters including extraction and desorption time, desorption solvent, ionic strength and pH value of sample matrix were investigated. The results showed that under the optimized experimental conditions, the method showed good sensitivity and excellent recoveries, as well as advantages such as linearity, simplicity, low cost and high feasibility. The extraction performance of present method to the target compounds also compared with commercial SBSE which using polydimethylsiloxane as coating and other SBSE which based on monolithic materials. Finally, the proposed method was successfully applied to the determination of PAAs in lake and sea waters, and excellent recoveries of spiked target compounds in real samples were obtained.     

Development and validation of stir bar sorptive extraction of polar phenols in water followed by HPLC separation in poly(vinylpyrrolididone‐divinylbenzene) monolith

An effective and simple method for polar phenols in water matrix was developed by using stir bar sorptive extraction (SBSE) based on a hydrophilic poly(vinylpyrrolididone‐divinylbenzene) (VPDB) monolithic material and HPLC analysis. To achieve optimum extraction performance for phenols, several parameters, including extraction and desorption time, desorption solvent, pH value, and ionic strength of sample matrix, were investigated. Under the optimized experimental conditions, eight phenols were directly enriched from water samples and analyzed by HPLC‐DAD. The detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target compounds were achieved within the range of 0.72–1.37 and 2.40–4.27 ng/mL from spiked water, respectively. Recoveries of eight phenolic compounds were found in the range of 55.2–95.9%. The calibration curves showed the linearity ranging from 5 to 150 ng/mL with linear regression coefficient R² values above 0.98. Method repeatability presented as intra‐ and interday precisions were also found with the RSDs less than 4.10 and 7.61%, respectively. The distribution coefficients between VPDB and water (K_VPDB/W) for phenolic compounds were also calculated and compared with K_O/W. Finally, the proposed method was successfully applied to the determination of the target compounds in tap water, sea water and wastewater samples.     

Stir rod sorptive extraction with monolithic polymer as coating and its application to the analysis of fluoroquinolones in honey sample

A stir rod sorptive extraction (SRSE) with monolithic polymer as coating was proposed to avoid the friction loss of coating during the stirring process. In our study, poly(2-acrylamide-2-methylpropanesulfonic acid-co-octadecyl methacrylate-co-ethylene glycol dimethacrylate) [poly(AMPS-co-OCMA-co-EDMA)] monolithic polymer was used as a coating of SRSE. The effect of concentration of porogen on SRSE performance was studied. Four fluoroquinolones (FQs) were selected as testing analytes to evaluate the extraction efficiency of SRSE. To achieve the optimum extraction conditions of SRSE towards FQs, several parameters, including extraction time, extraction temperature, stirring rate, sample solution pH and contents of inorganic salt in the sample solution were investigated. Under the optimized conditions of SRSE, a method for the determination of FQs in honey sample was proposed based on the combination of SRSE with liquid chromatography and electrospray ionization mass spectrometry (SRSE/LC/ESI-MS). The detection limits (LODs) of the proposed method for four FQs ranged from 0.06 to 0.14 ng/g and the recoveries were in the range of 70.3–122.6% at different concentrations for honey samples. Good method reproducibility was found as intra- and inter-day precisions, yielding the relative standard deviations less than 11.9% and 12.4%, respectively. The results show that SRSE with poly(AMPS-co-OCMA-co-EDMA) monolithic polymer as coating possessed good extraction capacity towards FQs in honey samples. Finally, the monolithic polymer coated stir rod was demonstrated to be reused at least 60 times.     

A new anionic exchange stir bar sorptive extraction coating based on monolithic material for the extraction of inorganic anion

A novel anionic exchange stir bar sorptive extraction (SBSE) coating based on poly(2-(methacryloyloxy)ethyltrimethylammonium chloride-co-divinylbenzene) monolithic material for the extraction of inorganic anion was prepared. The effect of preparation conditions such as ratio of functional monomer to cross-linker, content of porogenic solvent on the extraction efficiencies were investigated in detailed. The monolithic material was characterized by elemental analysis, scanning electron microscopy and infrared spectroscopy. In order to investigate the extraction capacity of the new coating for inorganic anion, the new SBSE was combined with ionic chromatography with conductivity detection, Br⁻, NO₃⁻, PO₄³⁻ and SO₄²⁻ were selected as detected solutes. Several extractive parameters, including pH value and ionic strength in sample matrix, desorption solvent, extraction and desorption time were optimized. The results showed that strongly ionic strength did not favor the extraction of anlaytes. Under the optimum experimental conditions, low detection limits (S/N = 3) and quantification limits (S/N = 10) of the proposed method for the target anions were achieved within the range of 0.92–2.62 and 3.03–9.25 μg/L, respectively. The method also showed good linearity, simplicity, practicality and low cost for the extraction inorganic anions. Finally, the proposed method was successfully used to detect the two different trademarks of commercial purified water with satisfactory recovery in the range of 70.0–92.6%. To the best of our knowledge, this is the first to use SBSE to enrich inorganic anions.     

Stir bar sorptive extraction coupled to liquid chromatography for the analysis of strobilurin fungicides in fruit samples

A stir bar microextraction (SBSE) procedure for the determination of seven strobilurin fungicides in fruit samples using liquid chromatography (LC) and diode array detection (DAD) has been developed. The samples were sonicated in the presence of ethanol before submitting the extracts to SBSE. The incorporation of drazoxolon as an internal standard before SBSE allowed calibration without the need to use the standard additions method. Under the optimized conditions, detection limits were in the 0.3–2 ng g⁻¹ range, corresponding to trifloxystrobin and metominostrobin, respectively. The SBSE–LC–DAD procedure showed good repeatability (RSD below 11% in all cases) and provided recoveries of 80–105% from spiked samples. The method was applied to fifteen fruit samples, and low levels of pyraclostrobin and trifloxystrobin were found in two of them.     

Poly (methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary for in-tube solid phase microextraction coupled to high performance liquid chromatography and its application to determination of basic drugs in human serum

A poly (methacrylic acid-ethylene glycol dimethacrylate) monolithic capillary column was prepared for in-tube solid-phase microextraction. Comparing with the commonly used open tubular extraction capillary, which cannot provide sufficient extraction efficiency since the ratio of its coating volume to that of the capillary void volume is relatively small, the monolithic column with greater phase ratio combined with convective mass transfer provides the possibility to improve the extraction efficiency with shorter capillary. As to poly (methacrylic acid-ethylene glycol dimethacrylate), its hydrophobic main chains and acidic pendant groups make it a superior material for extraction of basic analytes from aqueous matrix.An on-line monolithic capillary column solid phase microextraction (SPME) method was developed for determination of theobromine, theophylline and caffeine in serum samples. The high extraction efficiency was obtained for all the three analytes, yielding the detection limits of 12, 8 and 6.5 ng/mL by UV detection, respectively. Excellent method reproducibility (R.S.D. < 2.9%) was found over a linear dynamic range of 0.05-2 μg/mL in serum sample. The monolithic capillary column was proved to be reusable in coping with serum samples, which would facilitate practical determination of basic drugs.     

Study on miscibility of poly(vinyl chloride) and polyepichlorohydrin by viscometric and thermal analysis

Viscometric analysis was carried out to study the miscibility of poly(vinyl chloride) (PVC) and polyepichlorohydrin (PECH) in various solvents, tetrahydrofuran (THF), methyl ethyl ketone (MEK) and dimethylformamide (DMF). The Krigbaum–Wall criterion is used here to evaluate the miscibility of the two components, and Δb is introduced which can be calculated from the viscosity curves. The results show that their attractive forces are predominant when dissolved in THF, while in MEK and DMF repulsive forces play a leading role. This is attributed to different solubilities of the two polymers in the three solvents and to different influences of the solvents on the conformation of the polymers. Thermal measurement was performed by differential scanning calorimetry to investigate the glass transition temperature (T_g) of the blends prepared from the three solvents. Phase separation is observed for the samples made from MEK and DMF, while for THF the sample exhibits a single phase.     

Determination of steroid sex hormones in wastewater by stir bar sorptive extraction based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material and liquid chromatographic analysis

In this study, a simple and rapid method was developed for the determination of seven steroid hormones in wastewater. Sample preparation and analysis were performed by stir bar sorptive extraction (SBSE) based on poly(vinylpyridine-ethylene dimethacrylate) monolithic material (SBSEM) combined with high-performance liquid chromatography with diode array detection. To achieve the optimum extraction performance, several main parameters, including extraction and desorption time, pH value and contents of inorganic salt in the sample matrix, were investigated. Under the optimized experimental conditions, the method showed good linearity and repeatability, as well as advantages such as sensitivity, simplicity, low cost and high feasibility. The extraction performance of SBSEM to the target compounds also compared with commercial SBSE which used polydimethylsiloxane as coating. Finally, the proposed method was successfully applied to the determination of the target compounds in wastewater samples. The recoveries of spiked target compounds in real samples ranged from 48.2% to 110%.     

A sol-gel immobilization of nano and micron size sorbents in poly(dimethylsiloxane) (PDMS) microchannels for microscale solid phase extraction (SPE)

Sorbent particles consisting of nano and micro silica, and micron size octadecylsilica (ODS) were immobilized using sol-gel chemistry onto poly(dimethylsiloxane) (PDMS) microfluidic channels to serve as μ-chip solid phase extraction (SPE) devices. Extraction, preconcentration and purification of biological and chemical analytes were carried out using these. Micro and nano scale silica-immobilized μ-SPE were used for the extraction/purification of DNA from recombinant Escherichia coli crude lysate. The average DNA recovery was 77 ± 9% (X ± R.S.D.) for the micron size silica particles and 70 ± 5% (X ± R.S.D.) for the nano silica particles. The extracted DNA could be amplified by polymerase chain reaction (PCR) whereas the DNA from the crude lysate solution could not be. This was a testimony to the purification capability of the μ-SPE device. ODS immobilized μ-SPE were used to study the extraction efficiency (EE) and enhancement factor (EF) for three groups of organic compounds, aromatics, phenols and carboxylic acids. They showed poor recovery and low enrichment because the analytes sorbed into the PDMS and were not quantitatively extracted.     

Preparation of magnetic poly(vinylimidazole‐co‐divinylbenzene) nanoparticles and their application in the trace analysis of fluoroquinolones in environmental water samples

Nanosized spherical magnetic poly(vinylimidazole‐co‐divinylbenzene) particles were synthesized and used as a sorbent for the enrichment of trace fluoroquinolones (FQs) from environmental water samples. A suspension polymerization procedure was used to prepare the sorbent. The magnetic sorbent was characterized by SEM, transmission electron microscopy, elemental analysis, and FTIR spectroscopy. Analysis of enrofloxacin, marbofloxacin, fleroxacin, lomefloxacin, and sparfloxacin in environmental water samples by the combination of the magnetic sorbent and HPLC with diode array detection was selected as a paradigm for the practical application of the new adsorbent. Several extraction conditions, including desorption solvent, extraction and desorption time, pH value, and ionic strength in sample matrix, were optimized. Results showed that the new sorbent had high affinity for FQs and could be used to extract them effectively. Under the optimum conditions, low detection (S/N = 3) and quantification (S/N = 10) limits were achieved for the target analytes, within the ranges of 0.20–1.46 and 0.68–4.84 μg/L, respectively. Method repeatability was achieved in terms of intra‐ and interday precisions, indicated by the RSDs, which were both <10.0%. The method also showed good linearity, simplicity, practicality, and environmental friendliness for the extraction of FQs. Finally, the developed method was successfully applied to the determination of FQs in lake water, surface water, and reservoir water samples. Acceptable recoveries of spiked target compounds in these water samples were in the range of 52.1–104.5%.     

金属-有机骨架MIL-101(Cr)掺杂聚合物整体柱的制备及其用于酚类化合物的在线固相萃取

制备了金属-有机骨架（MOF）MIL-101（Cr）掺杂聚合物整体柱，建立了在线固相萃取-高效液相色谱检测水中4-硝基苯酚、2-硝基苯酚、3-甲基苯酚和2，4-二氯苯酚的方法。考察了样品溶液pH值、上样时间、上样流速和解吸时间对酚类化合物萃取效果的影响。在最优萃取条件下，采用制备的整体柱检测水中酚类化合物，其富集因子高，线性范围宽，精密度好，检出限低，适用于水中酚类化合物的检测。制备掺杂聚合物整体柱是促进和拓宽MOFs在线固相萃取应用的有效方法之一。     

Microwave-assisted extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs) used to indoor air monitoring

A rapid and environmentally friendly methodology was developed for the extraction of pyrethroid insecticides from semi permeable membrane devices (SPMDs), in which they were preconcentrated in gas phase. The method was based on gas chromatography mass–mass spectrometry determination after a microwave-assisted extraction, in front of the widely employed dialysis method. SPMDs were extracted twice with 30 mL hexane:acetone, irradiated with 250 W power output, until 90 °C in 10 min, this temperature being held for another 10 min. Clean-up of the extracts was performed by acetonitrile–hexane partitioning and solid-phase extraction (SPE) with a combined cartridge of 2 g basic-alumina, deactivated with 5% water, and 500 mg C₁₈.

Pyrethroids investigated were Allethrin, Prallethrin, Tetramethrin, Bifenthrin, Phenothrin, λ-Cyhalothrin, Permethrin, Cyfluthrin, Cypermethrin, Flucythrinate, Esfenvalerate, Fluvalinate and Deltamethrin. The main pyrethroid synergist compound, Pyperonyl Butoxide, was also studied. Limit of detection values ranging from 0.3 to 0.9 ng/SPMD and repeatability data, as relative standard deviation, from 2.9 to 9.4%, were achieved. Pyrethroid recoveries, for spiked SPMDs, with 100 ng of each one of the pyrethroids evaluated, were from 61 ± 8 to 103 ± 7% for microwave-assisted extraction, versus 54 ± 4 to 104 ± 3% for dialysis reference method. Substantial reduction of solvent consumed (from 400 to 60 mL) and analysis time (from 48 to 1 h) was achieved by using the developed procedure.

High concentration levels of pyrethroid compounds, from 0.14 to 7.3 μg/SPMD, were found in indoor air after 2 h of a standard application.     

分子印迹固相萃取-高效液相色谱法测定饲料中莱克多巴胺

以莱克多巴胺为模板分子,丙烯酰胺为功能单体,乙二醇二甲基丙烯酸酯为交联剂,合成了对莱克多巴胺具有高选择性的分子印迹聚合物。考察了甲醇、乙腈、丙酮和氯仿-甲醇与三乙胺构成致孔剂合成的聚合物性能及其形貌特征。通过正交试验优化的聚合反应配方为: 1.0 mmol莱克多巴胺,4.0 mmol丙烯酰胺,20.0 mmol乙二醇二甲基丙烯酸酯,6.0 mL乙腈-三乙胺(30:1, v/v), 50.0 mg偶氮二异丁腈。建立的基于分子印迹固相萃取-高效液相色谱测定饲料试样中莱克多巴胺的方法,在0.50～100 mg/L质量浓度范围内有良好的线性关系(r=0.9994);饲料试样中1.0、10及100 mg/kg 3个添加水平的莱克多巴胺平均回收率大于80%;批内、批间测定的相对标准偏差小于10%;检出限(信噪比为3)达到0.1 mg/kg。该方法灵敏、可靠,用于饲料等复杂基质中莱克多巴胺检测的效果优于相关标准分析方法。     

聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯)搅拌棒吸附萃取与液相色谱-质谱联用检测牛奶中的磺胺类药物

将聚(甲基丙烯酸-乙二醇二甲基丙烯酸酯) (poly(MAA-co-EDMA))聚合物原位聚合于玻璃内插管外表面上,得到一种多孔聚合物涂层;将其作为搅拌棒吸附萃取的萃取介质,考察了其对磺胺类药物的萃取性能;最后将其与高效液相色谱-电喷雾质谱(HPLC-ESI-MS)联用,建立了一种牛奶中4种磺胺类药物的检测方法。在最佳条件下,牛奶中4种磺胺类药物的检出限(S/N=3)和定量限(S/N=10)分别为0.11～0.52 μg/L和0.35～1.72 μg/L。在1～500 μg/L的范围内峰面积与质量浓度具有良好的线性关系,日内、日间测定的相对标准偏差不高于11.3%。结果表明,该方法简便、灵敏度高且成本低,适合于牛奶中磺胺类药物的检测。     

亚胺连接的多孔共价有机骨架材料结合固相萃取-液相色谱-串联质谱检测蜂蜜中雌激素

以亚胺连接的多孔共价有机骨架材料(IL-COF-1)作为固相萃取的吸附剂,建立了液相色谱-串联质谱快速检测蜂蜜样品中痕量雌激素的方法。该研究选择雌二醇、己烯雌酚、雌三醇、β-雌二醇和炔雌醇5种雌激素作为目标分析物。在蜂蜜样品中添加雌激素,采用单因素优化法对影响萃取效果的重要因素进行优化,获得最佳条件:IL-COF-1用量为30 mg,样品流速为3 mL/min,样品溶液pH值为7,以5 mL的1%(v/v)氨水-甲醇溶液进行洗脱,流速为0.4 mL/min,萃取过程中不添加NaCl。采用高效液相色谱-三重四极杆质谱联用技术对提取物中的雌激素进行定量分析。以乙腈和5 mmol/L的乙酸铵溶液作为流动相进行梯度洗脱,经C18色谱柱分离,采用电喷雾离子源、质谱多反应监测和负离子扫描模式,实现了蜂蜜样品中5种雌激素的快速定性定量分析。在最佳条件下,方法验证结果中雌三醇、β-雌二醇和炔雌醇的线性范围为1~500 ng/g,雌二醇和己烯雌酚的线性范围为0.1~100 ng/g,相关系数(r)为0.9934~0.9972。检出限(S/N=3)为0.01~0.30 ng/g,定量限(S/N=10)为0.05~0.95 ng/g。添加50 ng/g 5种雌激素进行重复性实验,日内精密度相对标准偏差(RSD)为3.2%~6.6%,日间精密度RSD为4.2%~7.9%。基于IL-COF-1的固相萃取-液相色谱-串联质谱法具有快速准确、灵敏度高等特点,适用于蜂蜜中雌激素的分析和检测。将该方法应用于4个实际蜂蜜样品中雌激素的检测,均未检出目标物;在低中高3个水平下,5种雌激素的加标回收率为80.1%~115.2%,结果令人满意。     

Sulfonated poly(styrene‐divinylbenzene) modified with amines and the application for pipette‐tip solid‐phase extraction of carbendazim in apples

Sulfonated poly(styrene‐divinylbenzene) modified with five kinds of amine functional groups was applied to the determination of carbendazim in apple samples with a pipette‐tip solid‐phase extraction method. The structures of the polymers were characterized by scanning electron microscopy, Fourier transform infrared spectroscopy, and thermogravimetric analysis. Five different modifications of the solid‐phase extraction sorbent based on sulfonated poly(styrene‐divinylbenzene) were tested under static and pipette‐tip solid‐phase extraction conditions. The polymer modified with p‐methoxyaniline showed the best recognition capacity and adsorption amount for carbendazim. Under the optimum conditions, 3.00 mg of the adsorbent, 1.00 mL of ethyl acetate as washing solvent, and 1.00 mL of ammonia/acetonitrile (5:95, v/v) as elution solvent were used in the pretreatment procedure of apple samples. The calibration graphs of carbendazim in methanol were linear over 5.00–200.00 μg/mL, and the limits of detection and quantification were 0.01 and 0.03 μg/mL, respectively. The method recoveries of carbendazim were in the range of 91.31–98.13% with associated intraday relative standard deviations of 0.76–2.13% and interday relative standard deviations of 1.10–1.85%. Sulfonated poly(styrene‐divinylbenzene) modified with p‐methoxyaniline showed satisfactory results (recovery: 97.96%) and potential for the rapid purification of carbendazim in apple samples combined with the pipette‐tip solid‐phase extraction.     

Fabric phase sorptive extraction: A new sorptive microextraction technique for the determination of non-steroidal anti-inflammatory drugs from environmental water samples

Fabric phase sorptive extraction (FPSE) is a new, yet very promising member of the sorbent-based sorptive microextraction family. It has simultaneously improved both the extraction sensitivity and the speed of the extraction by incorporating high volume of sol–gel hybrid inorganic–organic sorbents into permeable fabric substrates. The advantages of FPSE have been investigated for the determination of four non-steroidal anti-inflammatory drugs, ibuprofen, naproxen, ketoprofen and diclofenac, in environmental water samples in combination with gas chromatography–mass spectrometry. Initially, the significance of several parameters affecting FPSE: sorbent chemistry, matrix pH and ionic strength were investigated using a mixed level factorial design (3¹ × 2²). Then, other important parameters e.g., sample volume, extraction kinetics, desorption time and volume were also carefully studied and optimized. Due to the high sorbent loading on the FPSE substrate in the form of ultra-thin coating and the open geometry of the microextraction device, higher mass transfer of the target analytes occurs at a faster rate, leading to high enrichment factors in a relatively short period of time (equilibrium times: 45–100 min). Under optimal operational conditions, the limits of detection (S/N = 3) were found to be in the range of 0.8 ng L⁻¹ to 5 ng L⁻¹. The enrichment factors ranged from 162 to 418 with absolute extraction efficiencies varied from 27 to 70%, and a good trueness (82–116% relative recoveries) indicating that the proposed method can be readily deployed to routine environmental pollution monitoring. The proposed method was successfully applied to the analysis of target analytes in two influent and effluent samples from a wastewater treatment plant and two river water samples in Spain.     

Bioanalysis of dried saliva spot (DSS) samples using detergent-assisted sample extraction with UHPLC-MS/MS detection

Dried saliva spot (DSS) sampling is a non-invasive sample collection technique for bioanalysis that can be potentially implemented at the patient's home. A UHPLC-MS/MS assay was developed using detergent-assisted sample extraction to quantify BMS-927711, a drug candidate in development for the treatment of migraines, in human DSS. By implementing DSS sampling at the patients' home, the bioanalytical sample collection for pharmacokinetic evaluation can be done at the time of the acute migraine attack without the need for clinical visits. DSS samples were prepared by spotting 15 μL of liquid saliva onto regular Whatman FTA™ DMPK-C cards and verified with a UV lamp (at λ 254 nm or 365 nm) during DSS punching. The 4-mm DSS punches in a 96-well plate were sonicated with 200 μL of [¹³C₂, D₄]-BMS-927711 internal standard (IS) solution in 20/80 MeOH/water for 10 min, followed by sonication with 50 μL of 100 mM NH₄OAc with 1.0% Triton-X-100 (as detergent) prior to liquid-liquid extraction with 600 μL EtOAc/Hexane (90:10). UHPLC-MS/MS was performed with an Aquity^® UPLC BEH C18 Column (2.1 × 50 mm, 1.7 μm) on a Triple Quad™ 5500 mass spectrometer. The assay was linear with a concentration range from 2.00 to 1000 ng mL⁻¹ for BMS-927711 in human saliva. The intra- and inter-assay precision was within 8.8% CV, and the accuracy was within ±6.7% Dev of the nominal concentration values. This UHPLC–MS/MS assay has been successfully applied to determine the drug's pharmacokinetics within a clinical study. For the first time, we observed BMS-927711 exposure in human DSS, confirming the suitability of this sampling technique for migraine patients to use at home. Detergent-assisted extraction with Triton-X-100 could be very useful in DSS or other dried matrix spot (DMS) assays to overcome low or inconsistent analyte recovery issues.