Determination of seven active components in Salvia miltiorrhiza herb by matrix solid phase dispersion combined with ion liquid extraction followed by high performance liquid chromatography

A low cost,rapid and sensitive preparation method of silica gel supported ionic liquid(SGSIL)combined with matrix solid phase dispersion(MSPD)followed by high performance liquid chromatography(HPLC)with ultraviolet detection(UV)is proposed,and it was applied to determine the seven active compounds in Salvia Miltiorrhiza herb.SGSIL and ionic liquid[BMIM]BF4 were used as the adsorbent and the green elution reagent in the MSPD procedure.Several extraction conditions including type of filler and elution solvent,the volume of elution solvent,material liquid ratio were optimized.Under the optimum conditions,the SGSIL-MSPD-HPLC method showed a low limit of detection(LOD,S/N=3)of 0.0122-0.8788μg/mL for standard solution,limit of quantification(LOQ,S/N=10)of 0.0406-2.9292μg/mL for standard solution,wide linear range from 1.56 to 2000μg/mL for all compounds for standard solution,correlation coefficients(r)of more than 0.9990,acceptable reproducibility(relative standard deviations,RSDs<3.54%),and precision of RSDs<3.36%for intra-day,RSDs<3.50%for inter-day.The satisfactory recoveries ranged from 96.4 to 102.5,with RSDs less than 3.45%.The developed SGSIL-MSPD method is easier and more suitable for the determination of the seven active compounds in Salvia Miltiorrhiza herb than the traditional ultrasonic extraction.It was an effective and efficient method for the extraction and quantification of the seven active compounds in traditional Chinese herbal samples.

Matrix Solid-phase Dispersion Extraction of Alkaloids from the Roots of Aconitum kusnezoffii Reichb

Matrix solid-phase dispersion（MSPD） was developed for the extraction of four alkaloids, including aconitine, mesaconitine, hypaconitine and deoxyaconitine, from the roots ofAconitum kusnezoffii Reichb. The determination of the analyte was carried out by high performance liquid chromatography with UV detection. The alkaline alumina was used as sorbent. The mixture of acetonitrile and water was used as elution solvent. Several extraction parameters, such as type of sorbent, the ratio of sample to solid support material, type of the elution solvent and the volume of the elution solvent were tested. Mean recoveries ranged from 93.16% to 102.73%, with relative standard deviations from 0.27% to 4.17%. With the extraction efficiency and time expenditure taken into account, MSPD extraction should be a comparatively good method.

Determination of Tebuconazole Residue in Apples and Vegetables by Matrix Solid Phase Dispersion-Gas Chromatography

[ Objective] The study aimed to determine tebuconazole residue in apples and vegetables using matrix solid phase dispersion-gas chro- matography （MSPD-GC）. [ Method] The effects of extraction and determination conditions on the detection of tebuconazole left in apples and veg- etables were analyzed, and the optimum extraction conditions were determined. [ Result] The recovery rate of tebucenazole was the highest when the ratio of a sample to florisil dispersant was 1 ： 4, and the mixture of hexane and acetone （ 1 ： 1 ） with total volume of 8 ml was as the eluant. Under the optimum conditions, the relative standard deviation （RSD） of the method was 4.9% -7.6%, and the detection limit was 0.1 tJg/g, while the re- covery rate of tebuconazole changed from 86.7% to 95. 2% . [ Conclusion] The method was simple, accurate, sensitive and applicable to the de- termination of tebuconazole in aaricultural Droducts.

Degradation Dynamics and Residue Analysis of Flubendiamide in Cabbage and Soil by Liquid Chromatography-Tandem Mass Spectrometry with Dispersive Solid Phase Extraction

To formulate a scientific basis for a reasonable spray dose and safe interval period of 20% flubendiamide water dispersible granule (WDG) on controlling vegetable pests, degradation dynamics of flubendiamide in cabbage and soil was analyzed in this study. Dissipation and residue of flubendiamide in 20% flubendiamide WDG in cabbage and soil under field conditions were investigated by liquid chromatography-tandem mass spectrometry with dispersive solid phase extraction. Results showed that the degradation dynamic equations of flubendiamide in cabbage and soil were based on the first-order reaction dynamic equations. The half-lives of the degradation of flubendiamide were 3.51 d to 3.96 d and 3.43 d to 3.87 d in the cabbage of Yangzhou and Jingzhou, respectively, and 4.42 d to 5.13 d and 4.37 d to 4.99 d in the soil of Yangzhou and Jingzhou, respectively. The terminal residues of flubendiamide in the cabbage of Yangzhou and Jingzhou were 0.0247 mg·kg-1 to 0.0393 mg·kg-1 and 0.0225 mg·kg-1 to 0.0273 mg·kg-1, respectively, when 20% flubendiamide WDG was applied at a dose of0.050g·m-2. Flubendiamide is safe to be applied in cabbage fields at the recommended dose.

Fast determination of multi-mycotoxins in corn by dispersive solid-phase extraction coupled with ultra-performance liquid chromatography with tandem quadrupole time-of-flight mass spectrometry

A fast analytical method for the simultaneous determination of 9 mycotoxins, including alfatoxins （B1, B2, G1, and G2）, fumonisins （B1, B2 and B3）, zearalenone, and deoxynivalenol in corn using dispersive solid-phase extraction method and ultra-performance liquid chromatography coupled to tandem quadrupole time-of-lfight mass spectrometry （UPLC-Q-TOF-MS） was developed and validated. Samples were extracted with acetonitrile-water （84：16, v：v, containing 1% acetic acid） using ultrasonic extraction. The extracts were puriifed with a dispersive SPE method using C18 as a cleaning agent. The ifnal clear extracts were dried by nitrogen blowing and subsequently redissolved in methanol-water （5：5, v：v）. The samples were then analyzed by UPLC-Q-TOF-MS with 0.1% formic acid in ammonium acetate-methanol as mobile phase. The mean recoveries were ranged from 68.0 to 120.0%, and the relative standard deviation （RSD） ranged from 0.18 to 6.29%. Limits of detections ranged from 0.05 to 50 μg kg？1, and limits of quantiifcation ranged from 0.1 to 200 μg kg？1, which were below the legal limits set by the European Union for the legislated mycotoxins. The developed method was applied to 130 corn samples. Among the mycotoxins studied, alfatoxins B1 and fumonisins B1, B2 and B3 were the most predominant mycotoxins, and their concentrations were 0–593.12, 0–2.01×104, 0–6.94×103 and 0–3.05×103 μg kg–1, respectively.

Determination of organochlorine pesticides from juice samples using magnetic biochar-based dispersive micro-solid phase extraction in combination with dispersive liquid-liquid microextraction

Analysis of pesticide residue levels in juice beverages is important to ensure safe consumption and avoid global trade concerns associated to pesticide contaminations.A simple,inexpensive and effective method was developed for the determination of organochlorine pesticides(OCPs)in bottled juice drinks using GC-MS.Sample pretreatment was performed using dispersive solid-phase microextraction(D-μ-SPE)for matrix desorption and dispersive liquid-liquid microextraction(DLLME)for analyte enrichment.In this study,an affordable and effective sorbent for the adsorption of OCPs from juice samples was synthesized from avocado seeds mixed with magnetic precursors for D-μSPE.The ground avocado seeds combined with a magnetic precursor nanocomposite were characterized using various instruments including scanning electron microscopy(SEM),X-ray diffraction(XRD),Fourier transform infrared spectroscopy(FTIR),and Brunauer-Emmett-Teller(BET)analysis.The solution obtained from D-μ-SPE desorption was used as a dispersant for the subsequent DLLME,which made the combination of D-μ-SPE with DLLME much easier.The effectiveness of the method was enhanced by optimizing the influential parameters in both D-μ-SPE and DLLME.Then after,the optimal values were determined for the real sample analysis.Accordingly,there was good linear dynamic range with a coefficient of determination(r2)≥0.9989.The limit of detection and quantification were 0.02–0.69 and 0.06–2.10 ng/L respectively.The method showed high enrichment factors ranging from 96 to 313 with recoveries of 87–100%.Intraday and interday precisions were≤4%.Compared with other reported methods,this method is a one-step,simple,cheap,fast,and environmentally friendly alternative and straightforward method for adsorbing organochlorine pesticides from sample solutions.These results demonstrates the high potential of the proposed method for the extraction and cleanup of contaminants in selected juices and other related samples.

Development of matrix solid-phase dispersion method for the extraction of short-chain chlorinated paraffins in human placenta

Chlorinated paraffins（SCCPs） are widely used worldwide, and they can be released into the environment during their production, transport, usage and disposal, which pose potential risks for human health. In this work, an efficient, reliable and rapid pretreatment method based on matrix solid-phase dispersion（MSPD） was developed for the analysis of short-chain CPs（SCCPs） in human placenta by gas chromatograph-electron capture negative ion low-resolution mass spectrometry（GC-ECNI-LRMS） and gas chromatography–quadrupole time-of-flight mass spectrometry（GC–QTOF-HRMS）. The MSPD-relevant parameters including dispersing sorbent,sample-to-sorbent mass ratio, and elution solvent were optimized using the orthogonal test.Silica gel was found to be the optimal dispersing sorbent among the selected matrices. Under the optimal conditions, 44% acidic silica gel can be used as the co-sorbent to remove lipid and eluted by the mixture of hexane and dichloromethane（7：3, V/V）. The spiked recoveries of the optimized method were 77.4% and 91.4% for analyzing SCCPs in human placenta by GC-ECNI-LRMS and GC–QTOF-HRMS, and the corresponding relative standard deviations were10.2% and 5.6%, respectively. The method detection limit for the total SCCPs was 36.8 ng/g（dry weight, dw） and 19.2 ng/g（dw） as measured by GC-ECNI-LRMS and GC–QTOF-HRMS,respectively. The concentrations of SCCPs in four human placentas were in the range of

基于响应面法的基质固相分散萃取土壤中有机磷阻燃剂

有机磷阻燃剂(OPFRs)被广泛添加于商业品和日用品中,由于具有环境持久性、生物富集性和潜在毒性,已成为一种新兴的持久性有机污染物。因此需要建立能准确定量环境中OPFRs的检测方法。该文基于基质固相分散萃取(MSPD),结合气相色谱-串联质谱(GC-MS/MS)法测定土壤中10种有机磷阻燃剂,筛选对OPFRs具有高选择性的吸附剂,最终确定MSPD最佳萃取条件。该文基于单因素分析法考察了常见吸附剂(C18、PSA、Florisil、石墨化炭黑(GCB)和多壁碳纳米管(MWCNT))及其用量、洗脱溶剂及其体积、研磨时间对OPFRs萃取效率的影响。在此结果基础上,进一步利用响应面法(RSM)考察了3个关键因素(吸附剂用量、洗脱剂用量和研磨时间)以及交互作用对OPFRs萃取效率的影响。最终确定最优条件:吸附剂GCB,用量0.3 g;洗脱溶剂乙酸乙酯,用量10 mL;研磨时间5 min,此时10种OPFR的萃取效率为87.5%。在GC-MS/MS的多反应监测模式(MRM)下,以13C-PCB208为内标物进行定量。10种OPFRs在6个浓度梯度下,获得较好的线性,相关系数大于0.998。该方法的LOD和LOQ分别为0.006~0.161 ng/g和0.020~0.531 ng/g。在最佳条件下,加标土壤中OPFRs的加标回收率为70.4%~115.4%,相对标准偏差(RSD)为0.7%~6.7%。将该方法用于苏州不同功能土壤中OPFRs的含量测定,结果表明电子厂和汽修厂土壤中OPFRs总含量显著高于稻田土和校园土,电子厂和汽修厂土壤中主要污染物为磷酸三(2-氯异丙基)酯(TCIPP)、三苯基氧化膦(TPPO)、磷酸三(2-氯乙基)酯(TCEP)和磷酸三(1,3-二氯-2-丙基)酯(TDCPP),它们在电子厂土壤中含量分别为5.30、4.44、4.54、4.20 ng/g,在汽修厂土壤中的含量分别2.70、3.93、7.60、5.04 ng/g。目前关于TPPO的土壤污染报道较少,该研究在苏州工业区土壤中检出了高浓度TPPO污染。该方法成功用于土壤中10种OPFRs的检测。

分散固相萃取净化-超高效液相色谱-串联质谱法测定蜂蜜中双甲脒、杀虫脒及其代谢物

该研究建立了分散固相萃取-超高效液相色谱-串联质谱(dispersive solid phase extraction-ultra-performance liquid chromatography,UPLC-MS-MS)检测蜂蜜中双甲脒、杀虫脒及其代谢物残留的分析方法。蜂蜜样品2 g加入10 mL水溶液充分混匀,经1%(体积分数)氨化乙腈超声辅助提取后离心,利用N-丙基乙二胺、C18、氨基键合硅胶混合材料进行分散固相萃取净化,采用ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)色谱柱分离,以甲醇和0.1%(体积分数)甲酸水溶液为流动相进行梯度洗脱,多反应监测模式正离子扫描分析。6种农药及其代谢物平均回收率为84.1%~113.8%,相对标准偏差为0.9%~6.0%,检出限为0.2~0.8μg/kg,定量限为0.7~2.5μg/kg。实验结果表明该方法快速简便、灵敏度高,适用于蜂蜜中双甲脒、杀虫脒及其代谢物残留同时分析。

磁性氮化碳复合材料的制备及其对磷酸化肽的富集

蛋白质的磷酸化在细胞信号传导和疾病发生发展中起着重要作用,但磷酸化的动态变化和低丰度的特点使得对其直接分析有着较大的困难。为了解决磷酸化肽难离子化、检测丰度低的瓶颈问题,本研究制备了一种磁性氮化碳复合材料,结合基质辅助激光解吸电离飞行时间质谱(MALDI-TOF-MS),建立了一种对复杂样品中低丰度磷酸化肽富集与分析的方法。采用电子显微镜、红外光谱分析及X射线衍射分析等手段对合成的磁性氮化碳材料进行表征。以酪蛋白酶解产物为实验模型,发现磁性氮化碳材料能够实现对磷酸化肽的高选择性富集和高灵敏度检测,检出限为0.1 fmol。选择脱脂牛奶、人唾液和人血清为实际分析样品,发现磁性氮化碳材料对微量蛋白生物样品中磷酸化肽的分析具有较高的应用潜力。

磁分散固相萃取-高效液相色谱法检测人体尿样中天麻素

建立了一种磁分散固相萃取技术结合高效液相色谱法,用于快速检测人体尿液样本中的天麻素。采用化学共沉淀法自组装制备磁性活性炭/大孔树脂三元复合材料(Fe_3O_(4)/AC/MR),并将该材料用作吸附剂,实现尿液样本中天麻素的分离富集。在最佳实验条件下,天麻素浓度与峰面积间呈良好线性关系,线性范围为3.0×10^(-2)~10.0μg·mL^(-1),线性相关系数为0.9994,检出限为5.4μg·L^(-1)。以模拟人体尿液作为实际样品进行加标回收验证,加标回收率为94.87%~106.3%,相对标准偏差(RSD)在2.8%-4.2%之间。本研究建立的方法简便、快速、有效,为生物样本中天麻素的分离提纯提供了新方法。

基于分散固相萃取-超高效液相色谱-串联质谱法的大豆农药残留测定研究

本研究建立了一种分散固相萃取-超高效液相色谱-串联质谱测定吡虫啉、烯啶虫胺等6种常见农药残留的方法。方法学验证结果显示,所有农药的标准曲线线性良好(R^(2)>0.999),方法灵敏度良好;加标回收试验中不同加标浓度的相对标准偏差均小于10%,验证了方法的稳定性和可靠性。应用此方法对20份市售大豆样品进行农药残留检测,结果显示所有样品中农药残留均未超出或远低于国家规定的最大残留限量,合格率为100%。

六方氮化硼应用于样品前处理的研究进展

近几年,六方氮化硼由于孔隙率高、比表面积大、机械强度高、化学稳定性好、亲水性好、生物相容性好等优点,作为前处理材料获得了广泛关注,已被用于生物化学、食品安全、环境污染等领域的样品前处理,是一种理想的吸附剂。目前已开发了多种基于六方氮化硼材料作为吸附剂的样品前处理技术,包括固相萃取、分散固相萃取、固相微萃取、磁性固相萃取、管内固相微萃取、分散固相微萃取等,可实现多氯联苯、罗丹明B、黄酮类化合物、多环芳烃等分析物的萃取富集。综述了六方氮化硼材料在样品前处理领域的应用进展,并对今后的发展方向进行了展望。

分散固相萃取-液相色谱-串联质谱法测定不同品种柑橘果实不同部位中3种柠檬苦素类似物的含量

提出了分散固相萃取-液相色谱-串联质谱法同时测定4个品种柑橘果实的4个部位(油胞层、白皮层、囊衣、果肉)中柠檬苦素、诺米林、黄柏酮含量的方法。取5.0 g均质后的样品,加入5 mL水,涡旋混匀后加入20 mL体积比5∶5的丙酮-乙腈混合溶液,混匀后超声提取10 min,离心5 min。用3 mL水活化2 g EMR-Lipid吸附剂,加至上清液中,涡旋30 s,加入5 g质量比1∶4的氯化钠-硫酸镁混合物和15 mg石墨化碳黑,迅速摇匀后离心1 min。吸取全部上清液,于40℃氮吹至近干,残渣用10.0 mL体积比9∶1的0.1%(体积分数,下同)甲酸溶液和乙腈的混合溶液复溶,过0.22μm滤膜,滤液按照优化的仪器工作条件测定。进行色谱分析时,以CAPCELL PAK ADME HR色谱柱作固定相,以不同体积比的0.1%甲酸溶液和乙腈的混合溶液作流动相进行梯度洗脱分离;进行质谱分析时,以电喷雾离子源正离子(ESI+)和多反应监测(MRM)模式检测。结果显示:3种柠檬苦素类似物的质量浓度在0.10~10.0 mg·L^(-1)内和对应的峰面积呈线性关系,检出限(3S/N)均为0.01 mg·kg^(-1);按标准加入法进行回收试验,回收率为83.1%~90.5%,测定值的相对标准偏差(n=6)为2.6%~5.6%;方法用于30个实际样品的分析,柠檬苦素类似物在不同品种柑橘果实及其不同部位中的含量分布差异显著,柚类品种中柠檬苦素类似物总测定值较高且主要分布在囊衣部位,其他品种主要分布在白皮层和油包层。

响应面优化分散固相萃取-超高效液相色谱-串联质谱法测定膨化食品中3种大麻酚类化合物的含量

采用单因素和响应面法优化净化剂和提取溶剂用量,提出了题示方法。取2 g粉碎后的膨化食品样品,依次加入10 mL水、10 mL乙腈、4 g无水硫酸镁和1 g氯化钠,涡旋振荡15 min,离心5 min。取2 mL上清液置于含有200 mg十八烷基硅烷键合硅胶(C_(18))和30 mg N-丙基乙二胺(PSA)的离心管中,涡旋2 min,离心5 min,上清液过0.22μm滤膜,滤液采用超高效液相色谱-四极杆/飞行时间质谱法(UHPLC-Q-TOF/MS)测定。滤液中的大麻二酚、大麻酚、四氢大麻酚在Agilent Extend C_(18)色谱柱上用不同体积比的0.1%(体积分数)氨水溶液和乙腈的混合溶液梯度洗脱分离,电喷雾离子源负离子模式电离,基质匹配法定量。结果显示:建立的三因素三水平响应面模型为二次回归方程,相关系数为0.9949,最优条件(C_(18)、PSA和乙腈用量分别为200 mg、30 mg和10 mL)下考察指标四氢大麻酚的回收率试验值(94.1%)和预测值(93.6%)吻合;3种目标物的质量浓度在5.0~200μg·L^(-1)内和对应的母离子峰面积呈线性关系,检出限(3S/N)均为10.0μg·kg^(-1);对阴性米饼进行3个浓度水平的加标回收试验,回收率为81.9%~94.1%,测定值的相对标准偏差(n=6)为3.9%~7.3%。方法用于米饼、饼干、薯片样品的分析,在1个进口饼干样品中检出了大麻酚(27.8μg·kg^(-1))、大麻二酚(113μg·kg^(-1))和四氢大麻酚(30.6μg·kg^(-1)),其他样品均未检出这3种目标物。

亲脂性匹配色谱分离-超高效液相色谱-串联质谱法测定果蔬中21种三唑类杀菌剂

为了提高农药残留的色谱分离效率和降低基质效应,本研究提出亲脂性匹配色谱分离,选取三唑类杀菌剂为研究对象,建立了果蔬中21种三唑类杀菌剂的超高效液相色谱-串联质谱(Ultra performance liquid chromatography-tandem mass spectrometry,UPLC-MS/MS)检测方法。样品经乙腈提取,盐析分相,分散固相萃取净化,选用与三唑类杀菌剂具有相近亲脂性的色谱柱进行分离,探究不同亲脂性烷基键合相对基质效应、回收率以及三唑杀菌剂和基质组分色谱分离的影响。结果表明,亲脂性匹配色谱分离能够提高色谱分离效率,改善三唑杀菌剂和基质组分的色谱分离,21种三唑杀菌剂的基质效应为-8.3%~4.7%,在5~250μg/L浓度范围内线性关系良好,决定系数R2≥0.999,平均回收率为91.4%~108.1%,定量限为0.5~3.5μg/kg。该检测方法能够有效降低基质效应,使用溶剂校准曲线进行定量即可获得满意的回收率,显著提高了检测效率,具有简便、准确、灵敏度高等特点,适用于果蔬中三唑杀菌剂的检测。所述亲脂性匹配色谱分离,为农药残留的液相色谱-串联质谱法分析中液相色谱柱的选择和基质效应的降低提供了方法参考。

基质全溶解-固相萃取-UPLC-MS/MS法分析聚酯纤维中阻燃剂

目的探索聚酯纤维中常见有机磷酸酯阻燃剂(磷酸三苯酯和三苯基氧化膦)的分析方法。方法通过完全溶解法将样品基质溶解,再采用商品化固相萃取柱PEP-2对提取的样品溶液进行进一步净化,结合UPLC-MS/MS技术测定5种聚酯纤维样品中的两种有机磷酸酯阻燃剂。结果在最优的条件下,建立的分析方法线性关系良好(r≥0.9958),灵敏度高,磷酸三苯酯和三苯基氧化膦方法检测限分别为0.08 ng·g^(-1)和0.014 ng·g^(-1),加标回收率范围为80.2%~104.6%,方法精密度RSD值低于8.8%。结论建立的分析方法准确度高、精密度好、无基质干扰、稳定可靠,为该类基质中痕量污染物的分析提供了新的策略。

分散固相萃取净化-超高效液相色谱-串联质谱法同时测定水果中7种链格孢霉毒素的含量

目的建立分散固相萃取净化-超高效液相色谱-串联质谱法快速、准确地同时检测水果中7种链格孢霉毒素的方法。方法试样用酸化乙腈提取,无水硫酸镁除水,氯化钠盐析,上层清液经C_(18)与石墨化碳黑分散固相萃取净化后,采用超高效液相色谱-串联质谱法测定,基质匹配标准溶液外标法定量。结果7种链格孢霉毒素在0.005~0.500mg/L范围内线性关系好(r^(2)>0.99),检出限为0.005mg/kg,定量限为0.01mg/kg,回收率在77.30%~114.34%之间,批内相对标准偏差为0.65%~14.81%,批间相对标准偏差为0.03%~18.59%。结论该方法简单、高效,精密度及准确度高,适用于水果中7种链格孢霉毒素的测定。

分散固相萃取/荧光检测法选择性富集和定量人体血浆中的α-细辛醚

该研究采用基于共价有机框架TpBD-Me_(2)(COF-TpBD-Me_(2))的分散固相萃取/荧光检测法对人体血浆中的α-细辛醚进行选择性富集和定量检测。优化了COF-TpBD-Me_(2)对α-细辛醚的最佳吸附条件,包括吸附剂质量浓度、吸附时间、pH值、解吸试剂和解吸时间。此外,还通过吸附等温线和吸附动力学实验阐明了吸附行为和机理。α-细辛醚在0.1~10µg/mL范围内呈良好的线性关系,相关系数(r^(2))大于0.999,检出限(LOD)为0.0025µg/mL。该方法对人体血浆中α-细辛醚的加标回收率为92.2%~98.0%,相对标准偏差为1.9%~3.8%。实验结果证明所建方法可选择性富集人体血浆中的α-细辛醚并实现准确定量。该方法为选择性富集和快速定量复杂生物基质中的药物活性成分提供了参考。

Fe_(3)O_(4)@AC的制备及其对甲苯磺酸瑞马唑仑分离分析研究

采用超声辅助法制备磁性活性炭复合材料(Fe_(3)O_(4)@AC)并用作磁分散固相萃取剂,同时与高效液相色谱法联用对甲苯磺酸瑞马唑仑进行了分离分析。实验结果表明,在最佳实验条件下,甲苯磺酸瑞马唑仑浓度与峰面积间呈良好线性关系,线性范围为0.005~1.000μg/mL,线性相关系数为0.999 5,检出限为3.5μg/L。以模拟人体尿液作为实际样品进行加标回收验证,加标回收率为86.1%~106.9%,相对标准偏差(RSD)在2.9%~7.2%之间。