固相萃取-超高效液相色谱-串联质谱法同时测定猪肉中20种精神药物残留

建立了固相萃取和超高效液相色谱-电喷雾串联质谱（UPLC-ESI-MS/MS）同时测定猪肉中20种精神药物残留的方法。样品采用碱性乙腈作为提取试剂,提取液经Oasis MCX固相萃取柱净化后,以含0.1%（v/v）甲酸的水溶液和乙腈作为流动相梯度洗脱,用C18色谱柱分离,正离子模式扫描,多反应监测模式检测。20种化合物在5~100 μg/L质量浓度范围内均呈良好的线性关系,线性相关系数均大于0.99,以S/N≥10计算方法的定量限为5 μg/kg。在空白猪肉中添加5、10和50 μg/kg水平的20种药物,其平均回收率为66.8%~97.2%,相对标准偏差（RSD）为4.2%~12.4%。本方法快速、准确、可靠,适用于猪肉中精神药物多残留的同时测定。     

固相萃取-高效液相色谱/串联质谱法测定大鼠血浆中二十二碳六烯酸

建立了固相萃取-高效液相色谱/串联质谱(SPE-HPLC-MS/MS)测定大鼠血浆中二十二碳六烯酸(DHA)的分析方法。血浆样品经C18固相萃取(SPE)小柱净化后,采用Thermo C18色谱柱分离,以0.2%甲酸水溶液和乙腈为流动相,等度洗脱,在电喷雾离子源负离子模式下,采用质谱选择反应监测(SRM)模式检测,外标法定量。结果表明:DHA在0.10~60.0μg/mL范围内具有良好的线性关系(r2=0.9990);检出限(S/N=3)为0.04μg/mL,定量限(S/N=10)为0.10μg/mL;在2、10、30μg/mL 3个添加水平下,其平均回收率为94.0%~106.9%,方法的相对标准偏差(RSD)在2.15%~3.12%之间。该方法简单、快速,准确度、灵敏度高,适用于大鼠血浆中DHA的分析检测。     

固相萃取-超高效液相色谱-串联质谱法测定工业染料中芳香胺

工业染料中的偶氮染料在柠檬酸缓冲液中用连二亚硫酸钠还原为芳香胺,所得芳香胺经ProElut AZO专用硅藻土柱提取,用乙醚洗脱,浓缩至近干后用甲醇定容。以UPLC BEH C18色谱柱为分离柱,以不同体积比混合的甲酸-水(0.1+99.9)溶液和甲醇为流动相梯度洗脱,采用电喷雾电离源正离子模式检测。方法的检出限(3S/N)在0.5～1.0mg.kg-1之间。24种芳香胺的平均回收率在71.8%～96.5%之间,相对标准偏差(n=5)均小于8.0%。     

固相萃取/超高效液相色谱-串联质谱法测定化妆品中12种合成着色剂

建立了固相萃取/超高效液相色谱-串联质谱法(SPE/UPLC-MS/MS)同时测定指甲油、眼影、唇膏等化妆品中12种合成着色剂(酸性紫49、颜料红57、颜料红53∶1、酸性黄36、结晶紫、罗丹明B、分散黄3、颜料橙5、苏丹红Ⅰ、苏丹红Ⅱ、苏丹红Ⅳ和溶剂蓝35)的分析方法。样品用四氢呋喃(THF)、二甲基亚砜(DMSO)和甲醇分步超声波辅助萃取,HLB固相萃取柱净化后,在Acquity UPLC BEH-C18(2.1 mm×50mm,1.7μm)色谱柱上分离,乙腈和0.05%甲酸溶液为流动相梯度洗脱,采用多反应监测(MRM)模式进行检测,基质外标法定量。结果表明:12种着色剂在6 min内均显示较好峰形,其线性范围为0.5~800μg·L-1,相关系数均大于0.99。定量下限(LOQ,S/N10)为1.4~2 000μg·kg-1。在指甲油、眼影和唇膏中分别添加0.025~20 mg·kg-1浓度的着色剂进行加标回收实验,测定回收率为60.8%~118.0%,相对标准偏差(RSD)为2.3%~10.8%。该方法快速、简便、灵敏,适用于油状、粉状及膏状化妆品中禁限用着色剂的定量和确证分析。     

固相萃取-超高效液相色谱串联质谱法测定水中13种苯胺类化合物

建立了固相萃取-超高效液相色谱串联质谱法测定水中13种苯胺类化合物。样品通过HC-C₁₈固相萃取小柱富集,洗脱后加入内标苯胺-D5进行氮吹浓缩,经HSS T3色谱柱(150 mm×2.1 mm,1.8μm)分离,采用多反应监测扫描模式,以内标法定量。13种苯胺类化合物在0.1～100μg/L(其中3-硝基苯胺为0.2～200μg/L)范围内与特征离子的色谱峰面积线性关系良好,相关系数均大于0.995,方法检出限为0.001～0.006μg/L,平均加标回收率为67.3%～117%,测定结果的相对标准偏差为3.77%～16.9%(n=6)。该法操作简单、稳定性好,能够满足实际水体中13种苯胺类化合物大批量样品分析的需求。     

固相萃取-超高效液相色谱-串联质谱法测定飞燕草中7种生物碱北大核心CSCD

建立了固相萃取技术(SPE)结合超高效液相色谱-串联质谱法(UPLC-MS/MS)同时测定飞燕草中7种生物碱的方法。采用单因素实验考察了固相萃取中各因素对飞燕草中7种生物碱萃取率的影响。最佳萃取条件为:乙醇作为提取溶剂,稀HCl调节pH值为6.0,PCX固相萃取柱净化,3%氨水甲醇溶剂洗脱。洗脱液采用ACQUITY UPLC BHEC_(18)柱(50 mm×2.1 mm×1.7μm),以乙腈-0.2%NH_(4)Ac为流动相进行UPLC-MS/MS分析,7种生物碱在1~100 mg/L范围内线性关系良好,相关系数均不低于0.982,检出限为0.02~0.45 mg/L,定量限在0.08~1.23 mg/L之间。样品中3个添加浓度水平(1、5、10 mg/L)回收率为95.9%~98.1%,相对标准偏差(RSD)不大于2.5%。采用该方法对6个产地的飞燕草进行了检测,样品中7种生物碱的含量在0.08~0.94 mg/g之间。结果表明,本文所建立方法准确性好,灵敏度高,操作简单快速,可满足飞燕草中生物碱检测的要求。     

固相萃取-超高效液相色谱-串联质谱法测定蜂产品中10种头孢类药物

建立了蜂产品中10种头孢类药物（头孢喹肟、头孢噻肟、头孢洛宁、头孢哌酮、头孢匹林、头孢氨苄、头孢乙腈、头孢拉定、去乙酰基头孢匹林、头孢唑林）含量的液相色谱-串联质谱测定方法。蜂产品样品中头孢类药物用乙腈-水（80：20,v/v）溶液提取,离心,上清液经Oasis PRIME HLB固相萃取柱净化,氮吹后复溶,进行液相色谱-串联质谱分析。采用Acquity BEH C18色谱柱,以0.1%（v/v）甲酸水溶液-甲醇体系作为流动相进行梯度洗脱,ESI源正离子模式电离,多反应离子监测模式（MRM）检测,基质校准外标法定量。结果表明,10种头孢类药物在一定浓度范围内峰面积与质量浓度的相关系数（r²）大于0.999,线性关系良好;检出限为0.15~1.5 μg/kg,定量限为0.50~5.0 μg/kg;在阴性蜂产品样品中的加标回收率为75.0%~89.8%,相对标准偏差（RSD）为1.4%~4.6%（n=5）。该方法检测周期短,准确度和精密度高,能满足多种蜂产品样品中头孢类药物的检测需要。     

固相萃取-高效液相色谱-质谱法测定污水中糖皮质激素

建立了同时测定污水中7种糖皮质激素的固相萃取-超高效液相色谱串联质谱的分析方法.利用单因素实验优化固相萃取影响因素:洗脱液、洗脱体积、水样pH值及淋洗液.在此基础上,进行L9(34)正交实验.通过直观分析和方差分析区分主次因素,确定了最佳固相萃取条件:洗脱剂为乙酸乙酯,洗脱剂用量为10 mL,pH=5.0,清洗剂为20％甲醇.7种糖皮质激素的检出限为1.56～10.59 ng/L;在20～100 ng/L的3个添加水平范围内的平均回收率为72.5％～101.4％,相对标准偏差(RSD)小于10.9％.     

固相萃取-超高效液相色谱-串联质谱法测定水产品中多种兽药的残留量

用乙腈-乙酸乙酯(3+2)混合液(15.0mL)作溶剂超声提取水产品样品(3.00g)中喹诺酮(QNL′s)及磺胺(SFM′s)两类兽药的残留物,离心后取10.00mL清液,用氨基固相萃取柱进行分离。相继用正己烷及乙腈洗去油脂及干扰物质,然后用甲醇和甲醇-乙酸(99+1)的混合液洗脱两类药物的残留。洗脱液在45℃蒸干,用乙腈和含0.1%(φ)甲酸的5mmol·L-1乙酸铵溶液(1+4)的混合液溶解残渣,并定容至1mL,按仪器工作条件进行气相色谱-质谱分析。以8种药物内标对上述两类兽药共14种进行定量。14种药物的线性范围均在30μg·kg-1以内,检出限(3S/N)均为1μg·kg-1。在2种水产品中加入混合标准溶液并按方法进行回收试验,测得回收率在81.2%~116%之间,测定值的相对标准偏差(n=6)在0.72%~9.8%之间。     

通过式固相萃取-超高效液相色谱-串联质谱法测定水产品中地西泮

建立了通过式固相萃取-超高效液相色谱-串联质谱测定水产品中地西泮残留量的分析方法。样品用乙腈直接提取,经Prime HLB通过式固相萃取柱(60 mg/3 mL)净化,以Acquity UPLC BEH C₁₈(100 mm×2.1 mm, 1.7μm)为色谱柱,甲醇-0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱。在多反应监测(MRM)、正离子电离模式下检测,采用基质匹配标准曲线外标法进行定量分析。结果显示:在0.1～10 ng/mL范围内,地西泮线性关系良好(r²>0.99)。在1.5、3.0和15.0μg/kg 3个加标水平下,地西泮的加标回收率为88.2%～101.1%,日间和日内精密度(RSD)均在10%以下。该法简便快速,灵敏度高,可用于水产品中地西泮的准确测定。     

Automated on-line in-tube solid-phase microextraction coupled with HPLC/MS/MS for the determination of butyrophenone derivatives in human plasma

This paper describes a fully automated on-line method combining in-tube solid-phase microextraction (SPME) in which sample clean-up and enrichment are conducted through an open tubular fused-silica capillary column and high-performance liquid chromatography (HPLC)/tandem mass spectrometry (MS/MS) detection for the determination of six butyrophenone derivatives (moperone, floropipamide, haloperidol, spiroperidol, bromperidol, and pimozide) in human plasma samples. The six butyrophenones were extracted by repeatedly aspirating and dispensing plasma sample solutions on a DB-17 capillary column (60 cm × 0.32 mm i.d., film thickness 0.25 μm). The analytes retained on the inner surface of the capillary column were then eluted into an acetonitrile-rich mobile phase using a gradient separation technique. Extraction efficiencies ranged from 12.7% to 31.8% for moperone, spiroperidol, and pimozide, and from 1.08% to 4.86% for floropipamide, haloperidol, and bromperidol. The regression equations for all compounds showed excellent linearity, ranging from 0.05 to 50 ng/0.1 mL of plasma, except for moperone and spiroperidol (0.01 to 50 ng/0.1 mL). The limits of detection and quantification in plasma for each drug were 0.03–0.2 and 0.1–0.5 ng/mL, respectively. The intra- and inter-day coefficients of variation for all compounds in plasma were not greater than 13.7%.     

高效液相色谱-质谱/质谱测定血浆中格列苯脲

本文建立了人血浆中格列苯脲的高效液相色谱-质谱/质谱(HPLC-MS/MS)分析方法。血浆中格列苯脲测定的线性范围是1~300 ng/mL;高、中、低三个浓度分析测定的精密度(RSD)<15%;格列苯脲和格列齐特(内标)绝对回收率均>80%。本方法灵敏、准确,重现性好,用于血药浓度的测定获得满意结果。     

液相色谱串联质谱测定蔬菜中残留的唑菌胺酯

唑菌胺酯(pyraclostrobin)俗称百泰,德国巴斯夫公司于1993年开发的兼具吡唑结构的甲氧基丙烯酯酯类菌剂~([1]),主要用于防治小麦、水稻、花生、葡萄、蔬菜、香蕉、 柠檬、咖啡、果树、核桃、蔬菜、茶树、烟草和观赏植物、草坪及其他大田作物上由子囊菌纲、担子菌纲、半知菌类和卵菌纲真菌引起的作物病害~([2]).     

超高效液相色谱-串联质谱法同时测定大鼠血浆中阿帕替尼与紫杉醇

建立了同时定量测定大鼠血浆中阿帕替尼和紫杉醇的超高效液相色谱-串联质谱(UPLC-MS/MS)方法,并应用于药动学研究。血浆样品经固相萃取(SPE)处理。色谱柱为Agilent Zorbax Eclipse Plus C18柱(100 mm×2.1 mm,1.8μm),流动相为乙腈-0.1%甲酸溶液,体积流量0.4 m L/min,柱温40℃,进样量为3μL。质谱采用电喷雾正离子源模式(ESI+),多反应监测模式(MRM)进行定量测定。阿帕替尼和紫杉醇在0.5~1 500μg/L范围内均呈良好的线性关系(r2≥0.998),最低定量下限(LLOQ)均为0.5μg/L,日内、日间精密度RSD≤8.4%,准确度为92.5%~107.1%,提取回收率为86.2%~95.1%,基质效应(86.6%~108.6%)不影响待测物血药浓度的测定。经方法学验证,该法快速灵敏,可同时对阿帕替尼和紫杉醇进行血药浓度监测,为临床联合用药研究提供了重要的分析手段。     

Determination of Osimertinib,Aumolertinib, and Furmonertinib in Human Plasma for Therapeutic Drug Monitoring by UPLC-MS/MS

The third-generation epidermal growth factor receptor tyrosine kinase inhibitors (EGFR-TKIs), osimertinib, aumolertinib, and furmonertinib represent a new treatment option for patients with EGFR p.Thr790 Met (T790 M)-mutated non-small cell lung cancer (NSCLC). Currently, there are no studies reporting the simultaneous quantification of these three drugs. A simple ultra-performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) method was developed and validated for the simultaneous quantitative determination of osimertinib, aumolertinib, and furmonertinib concentrations in human plasma, and it was applied for therapeutic drug monitoring (TDM). Plasma samples were processed using the protein precipitation method (acetonitrile). A positive ion monitoring mode was used for detecting analytes. D₃-Sorafenib was utilized as the internal standard (IS), and the mobile phases were acetonitrile (containing 0.1% formic acid) and water with gradient elution on an XSelect HSS XP column (2.1 mm × 100.0 mm, 2.5 µm, Waters, Milford, MA, USA) at a flow rate of 0.5 mL·min⁻¹. The method’s selectivity, precision (coefficient of variation of intra-day and inter-day ≤ 6.1%), accuracy (95.8–105.2%), matrix effect (92.3–106.0%), extraction recovery, and stability results were acceptable according to the guidelines. The linear ranges were 5–500 ng·mL⁻¹, 2–500 ng·mL⁻¹, and 0.5–200 ng·mL⁻¹ for osimertinib, aumolertinib, and furmonertinib, respectively. The results show that the method was sensitive, reliable, and simple and that it could be successfully applied to simultaneously determine the osimertinib, aumolertinib, and furmonertinib blood concentrations in patients. These findings support using the method for TDM, potentially reducing the incidence of dosing blindness and adverse effects due to empirical dosing and inter-patient differences.     

超高效液相色谱-串联质谱法测定纺织品中19种邻苯二甲酸酯

采用超高效液相色谱-串联质谱法(UPLC-MS/MS)测定纺织品中19种邻苯二甲酸酯(PAEs)类化合物。实验采用Waters C_(18)色谱柱(50×2.1 mm,1.7μm),以甲醇-0.1%甲酸溶液为流动相,流速为0.4μL/min,采用梯度模式洗脱;质谱采用正离子电离模式(ESI+),多反应监测模式(MRM)检测。19种PAEs在其线性范围内线性良好(r20.994),定量限(S/N=10)为0.1~0.5mg/kg,回收率为88.8%~112.6%,相对标准偏差(RSDs,n=6)为1.1%~10.9%。实验表明该方法检测速度快,灵敏度高,适合纺织品中增塑剂的检测。     

超高效液相色谱-串联质谱法测定牛肉中非衍生化的脱呋喃甲酰基头孢噻呋残留量

建立了牛肉中脱呋喃甲酰基头孢噻呋(DFC)的超高效液相色谱-串联质谱(UPLC-MS/MS)检测方法。牛肉样品经DTE-硼酸盐缓冲液提取,过HLB固相萃取小柱净化浓缩,甲醇洗脱,UPLC-MS/MS法测定,仪器检测程序总色谱时间仅为5 min。方法平均回收率为80.7%～89.6%;批内变异系数范围在5.2%～9.7%之间;批间变异系数范围在6.1%～11.4%之间;检测限为0.55μg/kg;定量限为1.82μg/kg。方法可用于牛肉样品中脱呋喃甲酰基头孢噻呋药物残留量的确证检测。     

Determination and metabolism of brexpiprazole following baicalin to rats by a novel developed UPLC-MS/MS

The prime purpose of this research currently being done was to set up an acceptable and high-operational ultra performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) method, which could simultaneously analyze the concentration levels of brexpiprazole, assisted medication for treating depression, and DM-3411, the principal metabolite of brexpiprazole in rats, and to examine the impact of baicalin on the metabolism of brexpiprazole in rats. After quick sample preparation using acetonitrile as a protein precipitating agent, the chromatograms of brexpiprazole, DM-3411 and aripiprazole (internal standard, IS) were successfully separated by Acquity BEH C18 (2.1 mm × 50 mm, 1.7 μm) column. The concentrations of the analytes were detected through a Xevo TQ-S triple quadrupole tandem by the positive ion scanning. The ranges of calibration curves for both brexpiprazole and DM-3411 were 0.5–100 ng/mL, and the approach represented fine linearity in the ranges. The lower limit of quantification (LLOQ) of brexpiprazole and DM-3411 could reach 0.5 ng/mL in the study. The range of intra-day and inter-day accuracy of the two analytes was between −10.6% and 12.3%, while the precision was ≤ 11.5%. The recovery rate of each compound was greater than 81.0%, and no obvious matrix effects were observable. In addition, the plasma sample quantitative detection of the compounds in the study remained stable under all conditions. Then, we used this assay to detect the plasma levels of brexpiprazole and DM-3411 from a herb-drug interaction investigation, in which 200 mg/kg baicalin remarkably increased the plasma concentration of brexpiprazole and changed brexpiprazole pharmacokinetics. This study will contribute to a better understanding of the pharmacokinetic properties of brexpiprazole when concurrent use with baicalin, and to an understanding of the unanticipated clinical risks.     

UPLC-MS/MS检测3种蔬菜中的11种农药

建立了使用超高效液相色谱-串联质谱(UPLC-MS/MS)快速有效测定甘蓝、豇豆以及菠菜三种蔬菜中11种常见农药残留的方法。蔬菜样品经乙腈提取,Cleanert-NH2固相萃取柱净化后,采用ACQUITY UPLC·BEH C18色谱柱分离,以电喷雾电离、多反应监测模式检测。考察了不同配比的甲醇-水组成的流动相对电离效率、分辨率和灵敏度的影响,研究了不同蔬菜样品中的基质效应。通过基质匹配标准曲线进行定量,11种农药在5~100μg·L-1范围内线性良好,线性相关系数r0.99,目标农药的检出限在0.05~0.5μg·kg-1之间,11种农药在0.01 mg·kg-1,0.05 mg·kg-1和0.10 mg·kg-1三个加标水平下的回收率为80%~120%,相对标准偏差为2.7%~16.3%。     

超高效液相色谱-串联质谱法快速测定化妆品中水杨酸

提出了超高效液相色谱-串联质谱法测定化妆品中水杨酸含量的方法。化妆品试样用甲醇溶解,振荡提取20 min,离心分离取上清液过ACQUITYTMBET C18色谱柱(2.1 mm×100 mm,1.7μm)并用乙腈和甲酸-水(0.3+99.7)溶液(体积比6比4)的混合溶液作为流动相进行分离,串联质谱法进行测定。采用正离子模式多反应监测,同位素内标法定量。水杨酸的线性范围为1.0~5.0×103μg.L-1,方法的检出限(3S/N)为0.15μg.L-1,测定下限(10S/N)为0.50μg.L-1。方法用于分析8种化妆品试样,回收率在97.3%~107.0%之间,相对标准偏差(n=5)在2.0%~3.8%之间。