超高效液相色谱-串联质谱法测定茶叶中高氯酸盐

目的建立一种使用同位素内标法定量测定茶叶中高氯酸盐的超高效液相色谱-串联质谱法(ultra performance liquid chromatography tandem mass spectrometry,UPLC-MS/MS)。方法茶叶样品经0.2%乙酸提取,高速离心,上清液用石墨炭黑柱净化,再经Thermo Acclaim TRINITY P1色谱柱分离,串联质谱法检测,内标法定量。结果高氯酸盐在0.25~50.0μg/L范围内线性关系良好,相关系数(r)为0.9991。加标浓度为0.05~0.80 mg/kg时,方法的平均回收率分别为在94.6%~110.2%,相对标准偏差为1.8%~9.6%。结论本方法前处理简单、灵敏度高、准确、可靠,适用于茶叶中高氯酸盐的测定。     

超高效液相色谱-同位素稀释质谱法测定食品中的泛酸

目的 建立一种快速准确测定食品中泛酸含量的方法。方法 样品中的泛酸用水提取,经乙酸锌溶液和亚铁氰化钾溶液除杂后,以乙腈和0.1%甲酸溶液为流动相,通过Waters HSS T3 C18柱(2.1 mm×100 mm,1.7 μm)梯度洗脱分离,流速0.3 mL/min,进样量2 μL,柱温35 ℃,用串联质谱检测,同位素内标法定量。结果 泛酸在10-600 μg/L浓度范围内具有良好的线性关系,相关系数为0.9999,方法检出限为0.025 mg/100 g,定量限为0.075 mg/100 g,精密度的相对标准偏差为1.6%~1.8%,3个加标水平的回收率在92.6%~105%之间,相对标准偏差为1.9%~3.8%。该方法与微生物法相比结果无明显差异,且测定时间短,与高效液相色谱法相比抗干扰能力强。结论 超高效液相色谱-同位素稀释质谱法操作简单,快速准确,适用于多种食品中泛酸的测定。     

超高效液相色谱-串联质谱法测定茶叶中的百草枯

文章建立了一种利用超高效液相色谱-串联质谱法测定茶叶中百苹枯含量的方法.茶叶样品使用甲醇-0.1 mol/L盐酸溶液(3:7,V/V)提取,经Poly-sery MCX柱净化后用超高效液相液相色谱-串联质谱进行测定.在5～100μg/L浓度范围内,百草枯的线性良好(R2=0.9991),方法定量限为0.01 mg/kg...     

超高效液相色谱-串联质谱法测定食品中高氯酸盐

目的建立食品中高氯酸盐的超高效液相色谱-串联质谱(UPLC-MS/MS)的测定方法。方法香辛料调味品用水提取,蔬菜、水果用乙腈-水(1∶1,V/V)提取,肉、禽、蛋、奶和水产品用乙腈-水(2∶1,V/V)提取,C_(18)柱(3 ml,200 mg)净化,以高氯酸根为内标定量,采用UPLC-MS/MS法测定。结果在0.3~20.0μg/L范围内,3种提取溶液中高氯酸盐有良好的线性关系,R~2≥0.999。加标浓度在2.0~50.0μg/kg范围内,内标相对平均回收率为82.6%~108.6%,相对标准偏差(RSD)为1.0%~9.9%。牛奶的定量限为2.0μg/kg,其他食品的定量限为10.0μg/kg。结论本方法简单快捷,定量准确,适用于食品中高氯酸盐的测定。     

超高效液相色谱-串联质谱法同时测定食品中的氯酸盐和高氯酸盐残留量

目的 建立超高效液相色谱-串联质谱法测定食品中氯酸盐和高氯酸盐残留量的方法.方法 食品样品经纯水溶解,乙腈提取,固相萃取柱净化,排除复杂基体干扰,超高效液相色谱-串联质谱仪测定.采用多反应监测模式,电喷雾电离源负离子模式,内标法定量.结果 氯酸盐在0.5～200 ng/mL、高氯酸盐在0.1～100 ng/mL范围内线...     

超高效液相色谱-同位素稀释质谱法测定配方奶粉中的泛酸

建立测定配方奶粉中泛酸的超高效液相色谱-同位素稀释质谱方法。样品经乙酸铵溶液提取、三氯甲烷除 蛋白后,进行超高效液相色谱-串联质谱分析,采用HSS T3液相色谱柱分离,以10 mmol/L乙酸铵溶液（含0.1%甲 酸）和乙腈为流动相进行梯度洗脱,多反应监测模式,内标法定量。结果表明：方法定量限为0.040 mg/100 g,线 性范围内低、中、高3 个标准添加水平的回收率为96.9%～104.3%,相对标准偏差为3.78%～5.04%。该方法操作过 程简单、分析周期短、灵敏度高、重复性好,适用于奶粉中泛酸的测定。     

离子交换高效液相色谱-串联质谱法测定鸡肉和鸡肝中的高氯酸盐

建立测定鸡肉和鸡肝中高氯酸盐的离子交换高效液相色谱-串联质谱法。试样加18O标记高氯酸根离子后采用1%乙酸溶液-乙腈提取,固相萃取柱净化后,经IC-PakTM Anion HR （4.6 mm×75 mm ,6 μm）色谱柱分离,以乙腈-100 mmol/L乙酸铵溶液为流动相,采用电喷雾离子源串联质谱,在负离子扫描方式下以多反应监测模式检测,内标法定量。结果表明：高氯酸盐在0.2～10 μg/L质量浓度范围内线性关系良好,定量限为3.0 μg/kg。在3 个加标水平下的平均回收率为91.8%～96.0%,相对标准偏差为1.8%～6.5%。该方法操作简便、灵敏度高、抗干扰能力强、回收率和重复性良好,适用于鸡肉和鸡肝中高氯酸盐的测定。     

固相萃取-超高效液相色谱-串联质谱法测定土壤中的高氯酸盐

目的建立了一种同位素稀释超高液相色谱-串联质谱法测定土壤中高氯酸盐含量的分析方法。方法试样经0.2%乙酸水溶液和二氯甲烷提取,上清液经HLB小柱净化,液相色谱-串联质谱法测定,内标法定量。结果高氯酸盐在0.1～100μg/L浓度范围内线性关系良好,相关系数为0.9995,检出限为0.3μg/kg,定量限为1.0μg/kg,加标回收率在85.2%～102%,相对标准偏差(relative standard deviation, RSD)小于8.0%。结论该方法简便、可靠、稳定,可用于土壤中高氯酸盐含量的测定。     

稳定性同位素稀释-超高效液相色谱串联质谱法测定腐竹中的乌洛托品

采用超高效液相色谱-串联质谱法（UPLC-MS/MS）和稳定性同位素稀释技术,建立了测定腐竹中乌洛托品的分析方法。以乙腈为提取溶剂,向腐竹样品中加入乌洛托品的稳定性同位素,经固相萃取柱净化,采用HILIC色谱柱分离,目标物在UPLC-MS/MS的多反应监测（MRM）模式下,内标法定量。该方法在1⁴0μg/L范围内有良好的线性关系,相关系数为0.9996,方法定量限为2μg/kg。在添加水平为2、10、30μg/kg时,平均回收率为97.8%¹01.5%,相对标准偏差（RSD）为1.9%⁴.8%。本方法灵敏度高,准确度和重复性好,可为作为检测腐竹中违法添加乌洛托品的方法。      

超高效液相色谱-串联质谱法测定茶叶中6种农药残留

目的建立超高效液相色谱-串联质谱法测定茶叶中吡虫啉、多菌灵、啶虫脒、水胺硫磷、三唑磷和甲基异柳磷6种农药残留的方法。方法样品经乙腈提取,NH_2固相萃取小柱富集、净化,以二氯甲烷-甲醇(9:1,V:V)为洗脱溶液;样品经浓缩定容后,采用Thermo C_(18)(2.1 mm×50 mm,1.7μm)色谱柱分离,流速为0.3 mL/min,以水-甲醇-乙腈为流动相进行梯度洗脱,采用超高效液相色谱-串联质谱法多反应监测模式进行测定,采用基质标准溶液外标法定量。结果 6种农药在0.005~0.25μg/mL浓度范围内呈良好的线性关系,相关系数为0.9973~0.9998。当添加水平为0.005、0.025、0.25 mg/kg时,6种农药在茶叶中的加标回收率为72.4%~106.6%,相对标准偏差为1.6%~10.0%。方法定量限为0.5~5μg/kg。结论该方法操作简单、快速,可适用于茶叶中吡虫啉、啶虫脒、多菌灵、水胺硫磷、三唑磷和甲基异柳磷6种农药残留的测定。     

Determination of perchlorate in infant formula by isotope dilution ion chromatography/tandem mass spectrometry

A sensitive and selective isotope dilution ion chromatography/tandem mass spectrometry (ID IC-MS/MS) method was developed and validated for the determination of perchlorate in infant formula. The perchlorate was extracted from infant formula by using 20 ml of methanol and 5 ml of 1% acetic acid. All samples were spiked with (18)O(4) isotope-labelled perchlorate internal standard prior to extraction. After purification on a graphitised carbon solid-phase extraction column, the extracts were injected into an ion chromatography system equipped with an Ionpac AS20 column for separation of perchlorate from other anions. The presence of perchlorate in samples was quantified by isotope dilution mass spectrometry. Analysis of both perchlorate and its isotope-labelled internal standard was carried out on a Waters Quattro Ultima triple quadrupole mass spectrometer operating in a multiple reaction monitoring (MRM) negative ionisation mode. The method was validated for linearity and range, accuracy, precision, sensitivity, and matrix effects. The limit of quantification (LOQ) was 0.4 μg l(-1) for liquid infant formula and 0.95 μg kg(-1) for powdered infant formula. The recovery ranged from 94% to 110% with an average of 98%. This method was used to analyse 39 infant formula, and perchlorate concentrations ranging from 相似文献   

Analysis of pharmaceuticals in water by isotope dilution liquid chromatography/tandem mass spectrometry

A method has been developed for the trace analysis of 15 pharmaceuticals, four metabolites of pharmaceuticals, three potential endocrine disruptors, and one personal care product in various waters. The method employs solid-phase extraction (SPE) and liquid chromatography/tandem mass spectrometry (LC-MS/MS), using electrospray ionization (ESI) in both positive and negative modes. Unlike many previous LC-MS/MS methods, which suffer from matrix suppression, this method uses isotope dilution for each compound to correct for matrix suppression, as well as SPE losses and instrument variability. The method was tested in five matrices, and results indicate that the method is very robust. Matrix spike recoveries for all compounds were between 88 and 106% for wastewater influent, 85 and 108% for wastewater effluent, 72 and 105% for surface water impacted by wastewater, 96 and 113% for surface water, and 91 and 116% for drinking water. The method reporting limits for all compounds were between 0.25 and 1.0 ng/L, based on 500 mL of sample extracted and a final extract volume of 500 microL. Occurrence of the compounds in all five matrices is also reported.     

超高效液相色谱串联质谱法测定牛奶中三氮脒残留

目的 本研究旨在结合超高效液相色谱－串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)技术,建立简便、快速的样品前处理方法,对牛奶中的痕量三氮脒残留进行检测。方法 用1%乙酸乙腈溶液振荡提取后,在-4℃条件下高速离心,取上清液旋转蒸干后,用10%乙腈水溶液复溶,用超高效液相色谱-串联质谱仪在正离子扫描及多反应监测(multiple reaction monitoring, MRM)模式下分析,外标法定量。结果 牛奶中三氮脒的检出限(limit of detection, LOD)为5 μg/kg,定量限(limit of quantification, LOQ)为15 μg/kg,在20~1000 μg/L浓度范围内线性良好,相关系数(r)为0.9993。将所研究的方法应用于实际牛奶样本中,其加标回收率在81.65%至85.49%之间,日内精密度分别在4.5%~5.5%,日间精密度在5.9%~8.2%之间。结论 本方法采用振荡提取加低温高速离心净化的前处理方法,简单快速,结合UPLC-MS/MS,可实现痕量水平残留的高灵敏度检测,适用于快速、高灵敏检测牛奶及其他动物源性食品中的三氮脒残留。     

同位素稀释-超高压液相色谱-串联质谱法测定 维生素营养液中的泛酸含量

目的 建立测定维生素营养液中泛酸含量的同位素稀释-超高压液相色谱串联质谱法(ID-UHPLC-MS/MS)。方法 样品经高氯酸水溶液涡旋提取和除杂、超纯水稀释后,以HSS T3色谱柱和0.1%(v/v)甲酸水溶液-乙腈进行梯度洗脱分离,以串联质谱的多反应监测模式检测,内标法定量。结果 泛酸在5 ~1000 μg/L范围内具有良好的线性关系,相关系数(R₂)为0.9998;方法检出限为0.02 mg/100 g,定量限为0.07 mg/100 g;3个添加水平的回收率为92.5%~103%,相对标准偏差(n=6)为2.3%~5.2%;日间相对标准偏差(n=3)为2.72%。结论 本方法操作简便、分析速度快、灵敏度高、重复性好,为维生素营养液中泛酸含量的定性定量分析提供了可靠的依据。     

超高效液相色谱-串联质谱法测定生活饮用水中氯酸盐和高氯酸盐

目的 建立超高效液相色谱-串联质谱（UPLC-MS/MS）法同时测定生活饮用水中的氯酸盐和高氯酸盐的含量。方法 采用Anionic Polar Pesticide色谱柱（2.1 mm×150 mm,5 μm）为分析柱对高氯酸盐、氯酸盐进行分离,选用50 mmol/L甲酸铵甲酸水溶液（含0.9%甲酸）和乙腈作为流动相进行梯度洗脱。在电喷雾离子源,负离子多反应监测模式下测定,通过内标法进行定量。结果 氯酸盐和高氯酸盐在0.5～80 μg/L范围内线性关系良好,相关系数R2不低于0.999,氯酸盐和高氯酸盐的检出限、定量限均分别为0.5 μg/L和1.0 μg/L。氯酸盐和高氯酸盐均在1.0、2.0、20.0、80 μg/L 4个水平下回收率为83.98%～106.80%,相对标准偏差为0.57%～3.50% (n=6);结论 该方法简便、快捷、准确,适用于快速检测生活饮用水中的氯酸盐和高氯酸盐。     

Comparison of positive and negative ion detection of tea catechins using tandem mass spectrometry and ultra high performance liquid chromatography

Tea catechins are an important group of natural compounds associated with health promoting effects and desired commodities for the growing market of dietary supplements and functional foods. Consequently these compounds attract more interest of research groups worldwide. A reliable quantitative analysis of tea catechins is essential for human intervention studies, manufacturers of dietary supplements and quality control by authorities. UHPLC–ESI-MS/MS analytical method was chosen due to rapid runtime, high sensitivity and selectivity. The chromatographic separation of eight tea catechins was achieved within 2.5 min on C₁₈ BEH analytical column (100 mm × 2.1 mm i.d.; 1.7 μm), whilst the gradient elution mode was employed using water:methanol mobile phase with addition of volatile organic acid. The concentration of organic acids in the mobile phase was optimised within the range of 0.01–0.1% (v/v). High sensitivities were achieved in positive (10.2-16.8 fmol/inj.) and negative ion detection mode (102.1-168.1 fmol/inj.), through accurate and complex tuning of MS parameters. The UHPLC-ESI-MS/MS method was validated in terms of linearity (>0.9997; >0.9990), range (0.02–2.40 mg L⁻¹; 0.15-24.00 mg L⁻¹), LOD (3.0–4.8 μg L⁻¹; 30.1–48.0 μg L⁻¹), LOQ (9.9–15.8 μg L⁻¹; 150.5-240.0 μg L⁻¹), intra-day precision (4.4-7.1% RSD; 3.3-5.1% RSD), accuracy (94.06-113.7%; 89.5-108.4%), retention time repeatability (0.0-0.5% RSD; 0.0-0.6% RSD), and peak area repeatability (1.2-4.0% RSD; 2.4-3.5% RSD) for positive and negative ion detection modes, respectively. The statistical comparison of the quantitative results obtained in positive and negative ion detection mode was performed.     

液相色谱串联质谱法测定饲料中高氯酸盐含量

目的建立液相色谱串联质谱检测饲料中高氯酸盐含量的方法。方法饲料样品经乙腈-水(2:1,V:V)超声提取,高速离心后,上清液经石墨炭黑固相萃取柱净化,液相色谱串联质谱测定,内标法定量。结果高氯酸盐在0～100ng/mL浓度范围内呈良好线性关系(r2=0.9998)。本方法的定量限为15.0μg/kg。高氯酸盐在15～150μg/kg添加浓度范围内,回收率为95.1%～102.4%,相对标准偏差为1.13%～9.82%。结论本方法前处理简单,具有较高准确度、灵敏度、稳定性,可以满足饲料中高氯酸盐的含量检测。     

超高效液相色谱-串联飞行时间质谱法测定绿茶中9种拟除虫菊酯类农药

目的建立绿茶中9种拟除虫菊酯农药残留量检测的方法。方法采用超高效液相色谱电喷雾串联飞行质谱对9种拟除虫菊酯进行定量和裂解途径研究。结果样品经QuEChERS方法处理后上机,正离子模式下氟氯氰菊酯、氯氰菊酯、溴氰菊酯、氰戊菊酯、氟氰戊菊酯、四溴菊酯易形成[M+NH_4]~+加合离子,苯醚氰菊酯、甲氰菊酯、氟胺氰菊酯易形成[M+H]~+加合离子。采用一级母离子定量,9种拟除虫菊酯1～20μg/L范围内线性关系良好(r~20.99);9种拟除虫菊酯的最低检出限均为1μg/kg;2～10μg/kg范围内回收率为85.2%～106.3%;相对标准偏差(RSD)≤6.1%。结论方法简便、高效适用于绿茶中拟除虫菊酯类农药残留的快速筛查。