C_(18)膜萃取/液相色谱-质谱联用法测定极地水体中有机磷酸酯

建立了C_(18)膜萃取/液相色谱-质谱联用技术测定极地水体中10种有机磷酸酯(OPEs)的方法。根据优化后的样品前处理及仪器方法,利用C_(18)膜富集4 L水体中的10种OPEs,经二氯甲烷超声提取,在电喷雾正离子模式下,采用选择反应监测(SRM)模式进行分析,线性相关系数为0.994 4~0.999 9。10种OPEs的加标回收率为64.1%~115%,方法检出限为0.08~0.55 ng/L。该方法适用于极地水体中10种OPEs的分析,利用该方法对北极水体样品中的10种OPEs进行检测,测得冰川融水中∑OPEs的质量浓度为0.64~6.64 ng/L,海水中∑OPEs的质量浓度为0.09~2.03 ng/L。     

液液提取-固相萃取-高效液相色谱-串联质谱测定人体血液中16种有机磷酸酯

人体体液中有机磷酸酯(OPEs)浓度的测定对于了解人体OPEs的暴露水平以及评估人体健康风险具有重要意义.然而,目前的研究大多数集中于尿液中OPEs代谢物含量的分析测定,将其作为人体OPEs暴露的生物标志物,而对人体血液中OPEs的分析研究较少,仅有的少量研究涉及的OPEs种类有限.该研究在优化前处理过程(固相萃取,S...     

Sulfated and sulfonated polysaccharide as chiral stationary phases for capillary electrochromatography and capillary electrochromatography–mass spectrometry

The applications of polysaccharide phenyl carbamate derivatives as chiral stationary phases (CSPs) for capillary electrochromatography (CEC) are often hindered by longer retention times, especially using a normal-phase (NP) eluent due to very low electroosmotic flow (EOF). Therefore, in this study, we propose an approach for the aforementioned problems by introducing two new types of negatively charged sulfate and sulfonated groups for polysaccharide CSPs. These CSPs were utilized to pack CEC columns for enantioseparation with a NP eluent. Compared to conventional cellulose tris(3,5-dimethylphenyl carbamate) or CDMPC CSPs, the sulfated CDMPC CSP (sulfur content 4.25%, w/w) shortened the analysis time up to 50% but with a significant loss of enantiomeric resolution (∼60%). On the other hand, the sulfonated CDMPC CSP (sulfur content 1.76%, w/w) not only provided fast throughput but also maintained excellent resolving power. In addition, its synthesis is much more straightforward than the sulfated one. Furthermore, we studied several stationary phase parameters (CSP loading and silica gel pore size) and mobile phase parameters (including type of mobile phase and its composition) to evaluate the throughput and enantioselectivity. Using the optimized conditions, a chiral pool containing 66 analytes was screened to evaluate the enantioselectivity under three different mobile phase modes (i.e., NP, polar organic phase (POP) and reversed-phase (RP) eluents). Among these mobile phase modes, the RP mode showed the highest success rate, whereas some degree of complementary enantioselectivity was observed with NP and POP. Finally, the feasibility of applying this CSP for CEC–MS enantioseparation using internal tapered column was evaluated with NP, POP and RP eluents. In particular, the NP-CEC–MS provided significantly enhanced sensitivity when methanol was replaced with isopropanol in the sheath liquid. Using aminoglutethimide as model chiral analyte, all three modes of CEC–MS demonstrated excellent durability as well as excellent reproducibility of retention time and enantioselectivity.     

食品中有机磷酸酯阻燃剂检测技术的研究进展

有机磷酸酯(OPEs)是阻燃剂和塑化剂的主要原料,通常以添加形式存在于各种材料中,在生产和使用过程中伴随磨损和挥发易释放到环境中,现已成为新兴污染物。因为该类化合物的神经毒性、致癌性、破坏内分泌系统以及生殖系统等毒性,食品样品中OPEs的检测成为近年来关注的热点。该文重点围绕食品基质中OPEs检测存在的含量低、本底干扰严重、缺乏灵敏可靠分析方法等问题,对OPEs类化合物的性质、样品前处理、检测技术、质量控制等进行了全面评述。首先总结了30余种常见OPEs类化合物的类型、官能团、极性、沸点等理化性质,对可能的前处理和检测技术进行了理论分析;其次梳理了加速溶剂萃取(ASE)、基质固相分散萃取(MSPD)、微波辅助萃取(MAE)、超声辅助萃取(UAE)、QuEChERS、固相萃取(SPE)、凝胶渗透色谱(GPC)、分散固相萃取(d-SPE)等前处理方法在食品中OPEs化合物分析中的特点,其中UAE和QuEChERS结合多步净化能够有效降低高脂类食品的基质效应,具有良好应用前景;此外比较了气相色谱和液相色谱在分离和检测方面的优缺点,比较已有文献的检出限、回收率等数据;概括了标准品和内标物来源、过程污染与基质效应的产生原因和预防措施;最后对高分辨质谱筛查和鉴别OPEs未知代谢物,以及相关分析方法趋势进行了展望。     

Determination of two HMG-CoA reductase inhibitors, pravastatin and pitavastatin, in plasma samples using liquid chromatography-tandem mass spectrometry for pharmaceutical study

We developed a method for determining pravastatin or pitavastatin, 3-hydroxy-3-methylglutaryl coenzyme A (HMG-CoA) reductase inhibitors, in plasma using liquid chromatography and tandem mass spectrometry (LC-MS/MS). Pravastatin, pitavastatin and the internal standard fluvastatin were extracted from plasma with solid-phase extraction columns and eluted with methanol. After drying the organic layer, the residue was reconstituted in mobile phase (acetonitrile:water, 90:10, v/v) and injected onto a reversed-phase C(18) column. The isocratic mobile phase was eluted at 0.2 mL/min. The ion transitions recorded in multiple reaction monitoring mode were m/z 423 --> 101, 420 --> 290 and 410 --> 348 for pravastatin, pitavastatin and fluvastatin, respectively. The coefficient of variation of the assay precision was less than 12.4%, the accuracy exceeded 89%. The limit of detection was 1 ng/mL for all analytes. This method was used to measure the plasma concentration of pitavastatin or pravastatin from healthy subjects after a single 4 mg oral dose of pitavastatin or 40 mg oral dose of pravastatin. This is a very simple, sensitive and accurate analytic method to determine the pharmacokinetic profiles of pitavastatin or pravastatiny.     

Liquid chromatographic-electrospray tandem mass spectrometric determination of bisoprolol in human plasma

An analytical method for the determination of bisoprolol in human plasma has been developed based on liquid chromatography-tandem mass spectrometry (LC-MS/MS). The analyte and internal standard (IS) diphenhydramine were cleaned up by protein precipitation with acetonitrile, reconstituted in mobile phase and separated by reversed-phase high-performance liquid chromatography (HPLC) using methanol:10 mm ammonium acetate:formic acid (70:30:0.1 v/v/v) as mobile phase. Detection was carried out by multiple reaction monitoring (MRM) on an LC-MS/MS system and was completed within 2.5 min. The assay was linear over the range 0.5-100 ng/mL with a limit of quantitation (LOQ) of 0.5 ng/mL. The intra- and inter-day precision levels were within 5.54 and 9.95%, respectively, while the accuracy was in the range 89.4-113%. This method has been utilized in a pharmacokinetic study, where healthy volunteers were treated with an oral dose of 5 mg bisoprolol.     

Determination of sodium cromoglycate in human plasma by liquid chromatography with tandem mass

A sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed and validated for the determination of sodium cromoglycate (SCG) in human plasma after a nasal dose of 10.4 mg sodium cromoglycate nasal spray, using pravastatin sodium as the internal standard. The method was validated over a linear range of 0.300-20.0 ng/mL. SCG and I.S. were extracted from 1.0 mL of heparinized plasma by C(18) solid-phase extraction cartridges using methanol as eluting solvent. The dried residue was reconstituted with 100 microL of mobile phase, and 10 microL was injected onto the LC-MS/MS system. Chromatographic separation was achieved on a C(18) column (250 x 4.6 mm i.d., 5 microm particle size) with a mobile phase of methanol-acetonitrile-water (containing 2 mmol/L ammonium acetate; 42.5:42.5:15, v/v/v) at a flow rate of 0.4 mL/min. The analytes were detected with a triple quad LC-MS/MS using ESI with positive ionization. Ions monitored in the multiple reaction monitoring mode were m/z 469.0 (precursor ion) to m/z 245.0 (product ion) for SCG and m/z 447.2 (precursor ion) to m/z327.1 (product ion) for pravastatin sodium (internal standard) The average recovery of SCG from human plasma was 94.88% and the lower limit of quantitation was 0.3 ng/mL. Results from a 3-day validation study demonstrated excellent precision and accuracy across the calibration range of 0.3-20 ng/mL. The method was successfully applied to the pharmacokinetic study of SCG in healthy Chinese volunteers. Copyright (c) 2008 John Wiley & Sons, Ltd.     

Ultrasensitive determination of highly polar trimethyl phosphate in environmental water by molecularly imprinted polymeric fiber headspace solid‐phase microextraction

A sensitive, accurate, and cost effective method for the quantification of trimethyl phosphate, which is highly polar and volatile, in environmental water is presented. Trimethyl phosphate was headspace solid‐phase microextracted on a molecularly imprinted polymeric fiber, and then the fiber was thermally desorbed in the gas chromatograph injector, and the compound was determined. The trimethyl phosphate imprinted polymeric fiber was prepared by copolymerization in a fused silica capillary tube and obtained by removal of the wall of fused silica capillary tube. The monolithic fiber displayed good selectivity toward trimethyl phosphate among its structural analogues. It was thermally stable up to 320°C so that it can withstand the high temperature of the gas chromatograph injector for desorption. The factors influencing the performance of its headspace solid‐phase microextraction were studied. Under the optimal conditions, the method for quantification of trimethyl phosphate in environmental water was well developed. It exhibited significant linearity, the lowest limit of quantification to date, and good recoveries. Using this method, trimethyl phosphate was detected in five out of seven environmental water samples at concentration levels from 0.28 to 1.22 μg/L, illustrating the heavy pollution of trimethyl phosphate in environmental water.     

Liquid chromatography/tandem mass spectrometric bioanalysis using normal-phase columns with aqueous/organic mobile phases - a novel approach of eliminating evaporation and reconstitution steps in 96-well SPE

Bioanalytical methods using automated 96-well solid-phase extraction (SPE) and liquid chromatography with electrospray tandem mass spectrometry (LC/MS/MS) are widely used in the pharmaceutical industry. SPE methods typically require manual steps of drying of the eluates and reconstituting of the analytes with a suitable injection solvent possessing elution strength weaker than the mobile phase. In this study, we demonstrated a novel approach of eliminating these two steps in 96-well SPE by using normal-phase LC/MS/MS methods with low aqueous/high organic mobile phases, which consisted of 70-95% organic solvent, 5-30% water, and small amount of volatile acid or buffer. While the commonly used SPE elution solvents (i.e. acetonitrile and methanol) have stronger elution strength than a mobile phase on reversed-phase chromatography, they are weaker elution solvents than a mobile phase for normal-phase LC/MS/MS and therefore can be injected directly. Analytical methods for a range of polar pharmaceutical compounds, namely, omeprazole, metoprolol, fexofenadine, pseudoephedrine as well as rifampin and its metabolite 25-desacetyl-rifampin, in biological fluids, were developed and optimized based on the foregoing principles. As a result of the time saving, a batch of 96 samples could be processed in one hour. These bioanalytical LC/MS/MS methods were validated according to "Guidance for Industry - Bioanalytical Method Validation" recommended by the Food and Drug Administration (FDA) of the United States.     

Determination of N-methyl-4-isoleucine-cyclosporin (NIM811) in human whole blood by high performance liquid chromatography-tandem mass spectrometry

A liquid chromatographic method with tandem mass spectrometric detection (LC-MS/MS) for the determination of N-methyl-4-isoleucine-cyclosporin (NIM811) was developed and validated over the concentration range 1-2500 ng/mL in human whole blood using a 0.05 mL sample volume. NIM811 and the internal standard, d(12)-cyclosporin A (d(12)-CsA), were extracted from blood using MTBE via liquid-liquid extraction. After evaporation of the organic solvent and reconstitution, a 10 microL aliquot of the resulting extract was injected onto the LC-MS/MS system. Chromatographic separation of NIM811 and internal standard was performed using a Waters Symmetry RP-8 (50 x 4.6 mm, 3 microm particle size) column. The mobile phase consists of 10 mm ammonium acetate in water (A) and acetonitrile (B), with 45% B from 0 to 0.2 min, 45 to 85% B from 0.2 to 0.8 min and 85% B from 0.8 to 2.2 min. The total run time was 3.5 min with a flow rate of 0.8 mL/min. The method was validated for sensitivity, linearity, reproducibility, stability, dilution integrity and recovery. The precision and accuracy of quality control samples at low (2.00 ng/mL), medium (20.0 and 400 ng/mL) and high (2000 ng/mL) concentrations were in the range 1.1-4.3% relative standard deviation (RSD) and -2.5-10.0% (bias), respectively, from three validation runs. The method has been used to measure the exposure of NIM811 in human subjects.     

Development and validation of a hydrophilic interaction liquid chromatography-tandem mass spectrometric method for the analysis of paroxetine in human plasma

A sensitive, simple, fast and rugged hydrophilic interaction liquid chromatography-tandem mass spectrometry (HILIC-MS/MS) method for the determination of paroxetine was developed and validated over curve range 0.050-50 ng/mL using only 0.4 mL plasma. This is the first published LC-MS/MS method and the low limit of quantitation of this method is 10-fold lower than previously published methods. A simple liquid-liquid extraction method using methyl-tert butyl ether (MTBE) as the extraction solvent was used to extract paroxetine and the internal standard (IS) fentanyl-d(5) from plasma. The extract was evaporated to dryness, reconstituted and injected onto a silica column using a low aqueous-high organic mobile phase. The chromatographic run time was 2.0 min per injection, with retention times of 1.1 and 1.2 min for paroxetine and IS, respectively. The detection was by monitoring paroxetine at m/z 330 --> 192 and IS at m/z 342 --> 188, respectively. The inter-day precision and accuracy of the quality control (QC) samples were <5.0% relative standard deviation (RSD) and <2.9% relative error (RE). This method can be used for supporting therapeutical drug monitoring and pharmacokinetic or drug-drug interaction studies.     

MEKC–MS/MS method using a volatile surfactant for the simultaneous determination of 12 synthetic cannabinoids

This study describes a method for the simultaneous determination of 12 synthetic cannabinoids by MEKC–MS/MS using a volatile surfactant (ammonium perfluorooctanoate) as a constituent of the micellar pseudostationary phase. Although most synthetic cannabinoids comigrated by a CZE method, sufficient separation could be achieved by the proposed method. The best separation was made possible by 50 mM ammonium perfluorooctanoate in 20% v/v acetonitrile/water (apparent pH* 9.0) as the BGE, followed by MS detection using a sheath liquid composed of 5 mM ammonium formate in 50% v/v methanol/water mixed hydro‐organic solvent. The standard calibration curve for all analytes showed good linearity (r > 0.99). Satisfactory recoveries, ranging from 89.5 to 101.7%, were obtained. The LODs were 6.5–76.5 μg/g for the target analytes. This method appears to be a useful tool for the identification of synthetic cannabinoids in illegal herbal incense blends.     

Simultaneous Determination of Moxifloxacin Hydrochloride and Dexamethasone Sodium Phosphate in Rabbit Ocular Tissues and Plasma by LC-MS/MS: Application for Pharmacokinetics Studies

Treatment of ocular infection involves pharmacotherapy with steroids and antibiotic drops, such as moxifloxacin hydrochloride (MFH) and dexamethasone sodium phosphate (DSP). To characterize the pharmacokinetics of these two compounds, we performed and validated a liquid chromatography-mass spectrometry (LC-MS/MS) method to quantify them in rabbit ocular tissues and plasma. We used protein precipitation to extract the compounds. The analyte and internal standard (IS) were separated using a Shim-pack Scepter C₁₈ column. The mobile phase was composed of 0.1% formic acid water (A) and methanol (B). MFH and DSP were detected using positive ion electrostatic ionization (ESI) in multiple reaction monitoring mode (MRM). The calibration curves for both compounds showed good linearity over concentrations ranging from 0.5 to 200 ng/mL in rabbit ocular tissues and plasma. The lower limit of quantification for both MFH and DSP was 0.5 ng/mL. We validated this method for selectivity, linearity (r2 > 0.99), precision, accuracy, matrix effects, and stability. Thus, we used this method to assess the pharmacokinetic (PK) characteristics of MFH and DSP in rabbit ocular tissues and plasma after single doses. Our results indicate that this method can be used for the simultaneous analysis of moxifloxacin hydrochloride and dexamethasone sodium phosphate in clinical samples.     

Simultaneous determination of multiple intracellular metabolites in glycolysis, pentose phosphate pathway and tricarboxylic acid cycle by liquid chromatography-mass spectrometry

A highly selective and sensitive method for identification and quantification of intracellular metabolites involved in central carbon metabolism (including glycolysis, pentose phosphate pathway and tricarboxylic acid cycle) by means of liquid chromatography-tandem quadrupole mass spectrometry (LC-MS/MS) was developed. The volatile ion pair modifier tributylammonium acetate (TBAA) was employed in the mobile phase for simultaneously separation of 29 negatively charged compounds including sugar phosphates, nucleotides, and carboxylic acids on a common C18 reversed-phase column. Method validation results displayed that limits of detection (LODs) calculated according to DIN (German Institute for Standardization) 32645 are mostly below 60 nM, only with the exception of pyruvate and malate. The calibration curves showed excellent linearity mainly over three orders of magnitude with correlation coefficients R(2)>0.9982. This LC-MS/MS method was successfully applied to determine these metabolites in cell extracts of Escherichia coli. Most of the intracellular metabolites were found within the detection range and the relative standard deviations of the measurements were smaller than 5.65% (n=5) for a cell extract sample.     

Organophosphate esters in water,suspended particulate matter (SPM) and sediments of the Minjiang River,China

As organic pollutants of emerging concern, organophosphate esters (OPEs) have shown toxicity to organisms after entering the water environment. However, research on OPEs in freshwater in Southwest China is very limited. The levels, distribution and partitioning behavior of OPEs in the Minjiang River and their influencing factors is still unknown. In this study, six OPEs, tri-n-butyl phosphate (TnBP), tri(2-chloroethyl)-phosphate (TCEP), trichloropropyl phosphate (TCPP), triphenyl phosphate (TPhP), tributoxyethyl phosphate (TBEP), and tris(2-ethylhexyl)-phosphate (TEHP), were determined in surface water, suspended particle matter (SPM) and sediments of the Minjiang River. The results showed that the average concentrations of Σ₆OPEs in surface water, SPM and sediments of the Minjiang River were 199.32 ± 124.95 ng/L, 38463.79 ± 45641.89 ng/g dry weight (dw) and 76.45 ± 28.00 ng/g dw, respectively. High concentrations of OPEs were detected in SPM samples, indicating that more attention should be paid to pollution in SPM. It is worth noting that the variation trend of OPEs in SPM was almost opposite to that in water but basically similar to that in sediment. The proportions of alkyl OPEs in Σ₆OPEs increased from surface water to SPM and sediments. Alkyl OPEs were the main pollutants in SPM (10.44%–80.88% of Σ₆OPEs, mean of 54.52%) and sediments (59.08%–81.30% of Σ₆OPEs, mean of 68.91%), whereas chlorinated OPEs were the most abundant components in surface water (43.16%–75.99% of Σ₆OPEs, mean of 55.50%). The water-sediment partition coefficient (logK_OC) of OPEs was 4.97–7.58, while the water-SPM partition coefficient was 6.71–10.00. No significant correlations were found between logK_OW and logK_OC. K_OW was not the main factor affecting the distribution of OPEs in the Minjiang River, China.     

Analysis of polar peptides using a silica hydride column and high aqueous content mobile phases

The retention behavior of a set of polar peptides separated on a silica hydride stationary phase was examined with a capillary HPLC system coupled to ESI‐MS detection. The mobile phases consisted of formic acid or acetic acid/acetonitrile/water mixtures with the acetonitrile content ranging from 5 to 80% v/v. The effects on peptide retention of these two acidic buffer additives and their concentrations in the mobile phase were systematically investigated. Strong retention of the peptides on the silica hydride phase was observed with relatively high‐organic low‐aqueous mobile phases (i.e. under aqueous normal‐phase conditions). However, when low concentrations of acetic acid were employed as the buffer additive, strong retention of the peptides was also observed even when high aqueous content mobile phases were employed. This unique feature of the stationary phase therefore provides an opportunity for chromatographic analysis of polar peptides with water‐rich eluents, a feature usually not feasible with traditional RP sorbents, and thus under conditions more compatible with analytical green chemistry criteria. In addition, both isocratic and gradient elution procedures can be employed to optimize peptide separations with excellent reproducibility and resolution under these high aqueous mobile phase conditions with this silica hydride stationary phase.     

液相色谱-串联质谱法测定尿液中的内源性类固醇激素

建立了液相色谱-串联质谱(LC-MS/MS)测定尿液中的内源性类固醇激素的方法。尿样经葡萄糖醛酸甙酶酶解后进行液-液提取,以甲醇-0.1%甲酸缓冲液(含0.02 mol/L乙酸铵)(体积比为68:32)为流动相,采用Cosmosil C18色谱柱分离,并以三重四极杆串联质谱多反应监测扫描方式对尿样中的脱氢表雄酮(DHEA)、睾酮、表睾酮、雄酮和苯胆烷醇酮等5种激素进行检测。方法的最低检出限为0.01～10 ng/mL,平均回收率为96.7%～106.5%,日内和日间相对标准偏差(RSD)分别小于7%和11%。应用所建立的方法测定了健康志愿者口服DHEA后尿液中内源性类固醇激素的变化情况,结果表明该方法样品处理简便,色谱分离完全,结果准确可靠,可替代气相色谱-质谱法用于体液中内源性类固醇激素兴奋剂的常规分析。     

Rapid liquid chromatography-tandem mass spectrometry method for quantification of ziprasidone in human plasma

A liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the determination of ziprasidone (ZIP) in human plasma was developed. ZIP and N-methyl ziprasidone as internal standard (IS) were extracted from alkalinized plasma using tert- butyl methyl ether. Separation was performed isocratically on a C8 column with 90% acetonitrile containing 2 mmol/L ammonium acetate as a mobile phase with a total run time of 2.5 min. MS/MS transitions of m/z 413 --> 194 and m/z 427 --> 177 of the analyte and internal standard were used for quantification. Confirmatory ions of m/z 413 --> 177 and m/z 427 --> 180 were collected as well. The calibration curve based on peak-area ratio was linear up to at least 200 ng/mL with a detection limit of 0.1 ng/mL. The method showed satisfactory reproducibility with a coefficient of variation of less than 5%. The method was successfully applied to the analysis of ZIP in spiked human plasma.     

采用柱后抑制器技术降低流动相中三氟乙酸对质谱信号抑制作用的研究

研究柱后抑制器(CSRS)技术有效降低流动相中三氟乙酸(TFA)对质谱信号的抑制.采用双三元液相系统,左泵以反相模式分离细胞色素C酶解肽段(流动相含0.1%TFA,流速0.25 m L/min),柱后选择CSRS作为抑制器.同时右泵提供碳酸氢铵(浓度为0.05 mol/L,流速1.00 m L/min)作为再生液.碳酸氢铵和三氟乙酸在抑制器CSRS中通过阴离子交换膜进行离子交换,降低流动相中TFA离子抑制效应,提高肽段在质谱上的响应(S/N提高1~16倍).采用柱后抑制器技术对硫酸依替米星主成分及杂质进行定性分析(0.2 mol/L TFA),流动相经过抑制器后由强酸性变成中性,实现样品在LC和MS之间无缝连接分析.     

高效液相色谱-串联质谱法同时测定水体和沉积物中12种有机磷酸酯类化合物

建立了高效液相色谱-质谱联用技术结合固相萃取和液液萃取方法检测水体和沉积物中12种磷酸酯类(OPEs)化合物残留的方法.水样样品经HLB固相萃取柱富集,乙酸乙酯洗脱两次,沉积物样品以乙腈超声萃取,旋转蒸发至干,用超纯水稀释后重复水样处理步骤,采用ZORBAX Eclipse Plus C18色谱柱(150 mm×2.1 mm, 3.5 μm)进行分离,以0.2%甲酸-甲醇作为流动相进行梯度洗脱,采用正离子MRM监测模式,外标法定量分析.水样中,12种OPEs在0.05、0.10和0.50 μg/L加标水平下,除TMP (28.5%~47.8%)和TEHP (22.4%~73.8%) 外,其余目标化合物的平均回收率为66.4%~115.0%,相对标准偏差为0.5%~9.1%,方法定量限(MOQ)为0.001~0.050 μg/L;沉积物中,在5、10和50 μg/kg加标水平下,除TMP(35.7%~44.9%)、TCEP (31.2%~48.9%)外,其余目标化合物的平均回收率为65.9%~120.0%,相对标准偏差为0.01%~9.5%,方法定量限(MOQ)为0.02~2.0 μg/kg(dw).基于上述方法对太湖水样和沉积物样品中目标化合物定量检测分析,∑OPEs含量分别为0.1~1.7 μg/L和8.1~420 μg/kg dw.