高效液相色谱法测定口服液中低聚木糖的含量

建立了测定口服液中低聚木糖含量高效液相色谱法。样品中的大分子多糖和较高聚合度木糖用乙醇水溶液沉淀除去,然后用4.0mol/L硫酸水解,高效液相色谱测定,外标法定量。方法线性范围为0.1~4.0mg/mL(r=0.999);回收率:酸解前为100.1~103.1%,相对标准偏差RSD为1.0%(n=6)。酸解后为89.8~95.2%,相对标准偏差RSD为2.2%(n=6);检测限为10mg/mL。该方法选择性好,结果准确可靠,适用于口服液中低聚木糖含量的测定。     

气相色谱法测定口服液中肌醇的含量

建立了GC法测定口服液中肌醇含量的分析方法,该方法测定肌醇的线性范围为0.05~10.0mg/mL,检出限为0.001mg/mL,相对标准偏差(n=6)为0.51%,方法回收率为98.9~102.7%,并应用于口服液中肌醇的测定,结果良好。     

LC-MS/MS法测定Beagle犬血浆中ET-26盐酸盐及其代谢产物ET-acid

该文通过建立LC-MS/MS方法,采用全扫描离子(MRM)检测方式,测定静脉注射给药后Beagle犬中ET-26盐酸盐及其代谢产物依托咪酯酸的含量。采用色谱柱Agilent Extend-C18(3.0 mm×100 mm,3.5μm),流动相为水(0.01%NH3,用乙酸调pH至9.0)-乙腈,体积比35:65,采用ESI离子源,正离子模式下定量分析碎片离子质荷比(m/z)有ET-26盐酸盐275.3/105.1,依托咪酯酸m/z 217.0/113.1,依托咪酯杂质C(内标)m/z 259.0/155.1。ET-26盐酸盐与依托咪酯酸分别在3.225~2 090 ng/mL、3.253~2 108 ng/mL范围内,线性关系良好;定量限分别为3.225 ng/mL、3.253 ng/mL;检测限分别为0.97 ng/mL、1.00 ng/mL;日内、日间精密度RSD均小于15%;回收率分别在86.57%~105.03%、95.94%~98.27%范围内。该方法成功应用于Beagle犬中ET-26盐酸盐的药代动力学参数测定。结果表明该方法可以灵敏、有效地测定Beagle犬血浆中ET-26盐酸盐及其代谢产物依托咪酯酸的含量。     

微波辅助萃取-电感耦合等离子体质谱法检测食品中的硼砂

建立了一种应用微波辅助萃取-电感耦合等离子体质谱法检测食品中的硼砂的方法。以0.1 mol/L氨水来消除硼的记忆效应。硼含量在0～2.0μg/mL范围内线性关系良好,R=1.0000。硼砂检测限为2.0 ng/mL(σ=3),RSD小于5%,方法回收率为95.2%～103.4%。该法与GB/T21918-2008中的三种检测方法相比,具有操作简单、快速、试剂污染少的特点。可作为食品中硼砂含量的检测方法之一。     

高效液相色谱-荧光检测法检测金属食品罐用涂料中的双酚 A 含量

建立了一种高效液相色谱-荧光检测法测定金属食品罐用涂料中双酚 A 的定量分析方法。 样品用甲醇超声提取,双酚 A 在质量浓度为 0. 1 ~20. 0 μg/ mL 范围内,峰面积与质量浓度具有良好的线性关系,线性方程为 y=19. 241x+2. 7916,相关系数为 0. 9985,检测限为 0. 05 μg/ mL,回收率为 95. 0% ~100. 9% 。 分析比较了不同厂家和不同批号涂料中双酚 A 的含量。 研究表明,该方法灵敏可靠,准确度高,适用于定量检测金属食品罐用涂料中的双酚 A。     

高效液相色谱法测定桶装水及水桶中双酚A含量

该文建立固相萃取/高效液相色谱测定桶装水及水桶中双酚A含量的方法。桶装水样品经C18固相萃取柱富集,水桶用二氯甲烷溶解甲醇提取双酚A;采用C18色谱柱,以乙腈-水(V/V,60:40)为流动相,检测波长224 nm,高效液相色谱法测定双酚A含量。在最优检测条件下,双酚A在0.4～10μg/mL浓度范围内线性关系良好(r2=0.999 8),方法的检出限为0.069μg/mL,定量限为0.23μg/mL,平均回收率为98.3%。该方法简便、灵敏、重现性好,所抽取桶装水中并未检测到双酚A的存在,水桶材质中检测出双酚A的含量为37.1μg/g。     

环氧大豆油的合成工艺

目的 优化大豆油的环氧化工艺条件,提高大豆油的环氧化值。方法 采用浓硫酸作催化剂,将浓硫酸溶解于乙酸中,并混合均匀,加入大豆油中进行加热处理,同时滴加双氧水进行环氧化改性,通过测试产物的酸值和环氧值,研究双氧水用量、乙酸用量、浓硫酸用量和反应温度对大豆油环氧化效果的影响,并将该方式与常规方式进行对比。结果 当大豆油质量为100 g,质量分数为30%的双氧水用量为80 mL,乙酸用量为9 mL,浓硫酸用量为5 mL,反应时间为3 h,反应温度为60 ℃时,所合成的环氧大豆油的环氧值最高,为13.27 mol/(100 g),酸值为 0.081 mg/g（以KOH质量计）。结论 当乙酸用量过高时,会降低合成的环氧大豆油的环氧值;增加浓硫酸用量时,环氧大豆油的酸值会降低;温度升高则会提高其环氧值。所合成环氧大豆油的环氧值符合国家标准。     

顶空-气相色谱法测定卷烟主流烟气粒相物中吡啶

为研究气相色谱测定卷烟主流烟气粒相物中吡啶含量,采用碳酸钠水溶液作基质校正剂,通过顶空进样、DB-WAXETR色谱柱分离、火焰离子化检测器检测。结果表明:吡啶在0.20~16.20μg/mL质量浓度范围内线性拟合度为0.9998,加标回收率在98.4%~104.7%之间,定量限为0.08μg/支,RSD小于5%,该方法可以快速、准确地测定卷烟主流烟气粒相物中吡啶。     

药用胶塞常用抗氧剂及可提取硫含量测定方法

目的 建立一种高效液相色谱法，以同时检测药用胶塞中多种抗氧剂和可提取硫。方法 采用二氯甲烷作为提取溶剂，微波萃取药用胶塞中的目标化合物，用高效液相色谱法测定目标物的含量。色谱柱为Waters Symmetry RP 18，流动相为乙腈\甲醇\水，梯度洗脱，检测波长为277 nm。结果 该方法能高效地分离目标化合物，各化合物分离度良好。在0.2~20 μg/mL内线性良好，相关系数r≥0.999 3，检测限为0.03~0.09 μg/mL，回收率为86.73%～108.91%，相对标准偏差RSD为0.47%～5.68%。通过该种方法测定不同厂家不同批次药用胶塞，结果检出了抗氧剂BHT及其降解物BHT–CHO、BHT–Q，抗氧剂1076和1010及其降解物1310，以及可提取硫。结论 文中建立的高效液相方法准确、简便、灵敏度较高，能够高效快速地测定药用胶塞中常用抗氧剂及其降解产物与可提取硫的含量。     

UPLC同时测定决明子中橙黄决明素、大黄素、大黄酚和大黄素甲醚的含量

建立UPLC同时测定决明子中橙黄决明素、大黄素、大黄酚和大黄素甲醚含量的方法,采用ACQUITY UPLCBEH-C18色谱柱(2.1 mm×50 mm×1.7μm),乙腈和0.1%磷酸水溶液为流动相,采用梯度洗脱,流速为0.6 mL/min,检测波长为284nm。结果表明橙黄决明素、大黄素、大黄酚和大黄素甲醚分别在3.002～30.02μg/mL、2.500～25.00μg/mL、10.430～104.30μg/mL和5.916～59.16μg/mL的浓度范围内均有良好的线性关系(r=0.999 9),回收率均大于95%,RSD均小于2%。该方法快速,准确,重现性好,可用于测定决明子中橙黄决明素、大黄素、大黄酚和大黄素甲醚的含量。     

橄榄油中角鲨烯含量的气相色谱/质谱法分析

本文建立了橄榄油中角鲨烯含量的GC/MS分析方法.橄榄油中的脂肪酸甲酯化,角鲨烯同步萃取于石油醚-苯(1+1)溶剂中,经强极性毛细管柱SP-2560分离,质谱选择离子监测对角鲨烯进行定量测定.该方法在0.01-0.50mg/mL范围内线性关系良好,相关系数为0.9999,最小检测限为1.80ng/mL,方法回收率在99...     

肉桂油气相色谱与气质联用分析

目的:建立肉桂油中桂皮醛的含量测定方法和鉴定挥发性化学成分。方法:气相色潜法,3mm×4m不锈钢柱,10％PEG-20M为固定液,Chromosorb WAW 60-80目担体,FID检测器,柱温190℃;气质联用,以HP-5毛细管柱,柱温起始120℃保持5min后以5C/min升温至150(保持7min,检测质荷比范围10-425。结果:桂皮醛在2-10mg/mL范围内具良好线性关系,平均回收率为99.98％,RSD为1.3％,气质联用鉴定了39种化合物。结论:方法简便,快速,准确,可有效排除其它成分的干扰。     

丁香罗勒油气相色谱与气质联用分析

目的:建立丁香罗勒油中丁香酚的含量测定方法和鉴定挥发性化学成分。方法:气相色谱法,4mm×2m不锈钢柱,10％SE—30为固定液,Chromosorb WAW 60～80目担体,FID检测器,柱温110℃,水杨酸甲酯为内标物;气质联用,以HP—5毛细管柱,柱温起始120℃保持5min后以5℃/min升温至150℃保持7min,检测质荷比范围10～425。结果:丁香酚在2～10mg/ml范围内具良好线性关系,平均回收率为100.08％,RSD为0.95％;气质联用鉴定了39个化合物。结论:方法简便,快速,准确,可排除其它成分的干扰。     

液液萃取-GC/MS法分析地表水中的多氯联苯

建立了液液萃取-GC/MS联用分析地表水中的多氯联苯的方法,并对实际水样进行了测定。各目标物的线性回归R值均大于0.999,MDL为0.08-3.9ng/L,RSD为0.25%-6.2%,回收率为87.6%-113%。     

Speciation of inorganic lead and ionic alkyllead compounds by GC/MS in prescreened rainwaters

A simple and novel screening method for lead compounds in environmental waters is proposed. The analytes, in an acetic medium, are sorbed on a C60 fullerene column as diethyldithiocarbamate complexes and subsequently eluted with isobutyl methyl ketone (IBMK), the lead being determined by flame atomic absorption spectrometry. The screening method acts as filter and indicates whether the target analytes are present above or below the detection limit of the method (0.5 ng/mL), giving no false positives. Positive samples were speciated by GC/MS, using a flow system similar to that of the screening method. Lead(II) and ionic di- and trialkyllead are derivatized with a Grignard reagent. Both methods use similar chemical and flow variables except for the eluent, IBMK in the screening method and n-hexane in the speciation method. The GC/MS speciation method is very sensitive; it exhibits a linear range of 0.02-5 ng/mL, and detection limits of 1-4 ng/L are achieved. Also, its repeatibility, as RSD, is less than 6%. The method was applied to the speciation of Pb2+ and di- and trialkyllead in positive prescreened rainwater samples from three different urban areas.     

水浮莲叶挥发性化学成分的GC/MS法分析

采用气相色谱-质谱联用方法(GC/MS)分析了水浮莲叶中挥发性化学成分。以水蒸气蒸馏法从水浮莲叶中提取挥发油,以毛细管柱为分离柱,在最佳分析条件下共分离出30个化合物,用归一化法测定其相对含量,并用气相色谱-质谱法对分离出的化学成分进行鉴定,共鉴定了26个成分,占挥发油总成分的95·20%。该法对挥发油化学成分的分离效果满意。     

GC/MS with post-column switching for large volume injection of headspace samples: sensitive determination of volatile organic compounds in human whole blood and urine

When volatile or semivolatile compounds are measured by headspace (HS) gas chromatography (GC)/mass spectrometry (MS), the maximum gas volume to be injected is usually 0.5-1.0 mL; over the volume, the MS detector automatically shuts down due to impairment of the vacuum rate of the MS ionization chamber. To overcome the problem, we modified the gas flow routes of a new type of GC/MS instrument to create a postcolumn switching system, which can eliminate the large volume of gas before introduction of target compounds into the MS ionization chamber. Our HS-GC/MS system enabled injection of as large as 5 mL of HS gas without any disturbance. As the first example analysis, we tried to establish the analysis of naphthalene and p-dichlorobenzene in human whole blood and urine by this method with large volume injection. The limits of detection for both compounds in whole blood and urine were as low as about 10 and 5 pg/mL, respectively. The validation data and actual measurements were also demonstrated. The new GC/MS system has great potential to analyze any type of volatile or semivolatile organic compounds in biological matrixes with very high sensitivity and full automation.     

Ultrasensitive determination of phencyclidine in body fluids by surface ionization organic mass spectrometry

Gas chromatography (GC)/surface ionization organic mass spectrometry (SIOMS) has been found to give much higher sensitivity for measurements of phencyclidine (PCP) than the conventional GC/electron impact (EI)-mass spectrometry (MS). Thus, we have established a detailed procedure for measurements of PCP in body fluids by both mass chromatography and selected-ion monitoring (SIM) of SIOMS using pethidine as an internal standard (IS). Good linearity was found in the range of 0.25-10 ng/mL of whole blood or urine, when measured by mass chromatography, and in the range of 0.025-1.0 ng/mL of whole blood by SIM. The recoveries of PCP and IS spiked to whole blood were 106 +/- 17% at 1 ng/mL and 113 +/- 11% at 5 ng/mL; that of IS was 97.8 +/- 10.4% at 5 ng/mL. The detection limits (signal-to-noise ratio = 3) were estimated to be 0.05 ng/mL of whole blood or urine by mass chromatography and 0.01 ng/mL of whole blood by SIM. The coefficients of intraday and interday variations were not greater than 10.3%. We could detect PCP from rat whole blood 2 h after subcutaneous injection of PCP (1 mg/kg) by mass chromatography. The mean PCP concentration in rat blood was 47.7 +/- 6.2 ng/mL (mean +/- SD, n = 4).     

固相萃取-气相色谱-质谱联用法检测进出口蔬菜产品中百菌清残留

建立了固相萃取-气相色谱-质谱法检测蔬菜中百菌清残留的分析方法。样品用乙腈-水-磷酸混合液提取,经液液分配、Florisil/Na2SO4柱净化后过滤膜上机。采用选择离子扫描方式,外标法定量。通过优化前处理和上机条件,在最优条件下进行测试,实验结果百菌清的定量检出限为0.001mg/kg,在加标水平0.005～0.1mg/kg范围内,回收率为78.65%～90.67%,相对标准偏差为3.5%～5.8%。该方法简便、快速、净化效果理想,能满足残留分析的要求,可用于进出口蔬菜中百菌清残留的检测。     

Preparation and certification of standard reference material 1507: 11-nor-delta 9-tetrahydrocannabinol-9-carboxylic acid in freeze-dried urine

The National Institute of Standards and Technology (NIST) has prepared and certified SRM 1507, a freeze-dried urine fortified with 11-nor-delta 9-tetrahydrocannabinol-9-carboxylic acid (THC-9-COOH), the major urinary metabolite of marijuana. The certified concentration of 20 +/- 1 ng/mL for the analyte was obtained from the concordant results of analyses of the material by gas chromatography/mass spectrometry (GC/MS) and high-performance liquid chromatography with electrochemical detection (HPLC-EC). Solid-phase extraction was used to prepare the sample for GC/MS analyses, and liquid-liquid extraction was used for the HPLC-EC analyses. The multistep HPLC method was developed at NIST to circumvent interferences from urinary constituents. The results of a round robin test on this material among five Department of Defense laboratories involved in drug testing are reported.