高效液相色谱法同时测定染发剂中10种染料组分

建立了一种高效液相色谱法同时测定染发剂中对苯二胺等10种氧化型染料组分的检测方法.选用色谱柱Poroshell 120 Bonus-RP,针对对苯二胺、间苯二酚、对氨基苯酚、间氨基苯酚、4-氨基间甲酚、氢醌、4-氨基-2-羟基甲苯、2-硝基对苯二胺、甲苯-2,5-二胺硫酸盐和6-羟基吲哚等10种染料组分进行分析测定.方法在0.01~0.50 mg/m L质量浓度范围内线性相关系数为0.999 86~0.999 96,RSD小于5.91%,回收率为87.2%~106.7%.方法具有简单、快捷、分离效果好等特点.     

高效液相色谱法同时测定染发剂中8种合成染料

使用甲醇对样品进行超声提取,以乙腈-0.02 mol/L乙酸铵溶液为流动相,采用XB-C18色谱柱分离,二极管阵列检测器检测,外标法定量,建立了同时测定染发剂中8种合成染料的高效液相色谱分析方法。HC红3号、分散黑9、HC黄2号、分散紫1及HC橙1号的检测波长设为240 nm,HC黄4号设为410nm,HC蓝7号为450 nm,HC红1号为270 nm。8种染料在0.5~100.0μg/m L范围内具有良好线性,相关系数(r2)均不小于0.999 3。HC红3号、HC黄4号、HC橙1号和分散紫1的检出限均为0.70 mg/kg,分散黑9、HC黄2号、HC蓝7号和HC红1号的检出限分别为2.50,0.60,0.35,0.50 mg/kg。样品的平均回收率为85.4%~99.8%,相对标准偏差(n=6)为1.1%~3.6%。方法的精密度、准确度、回收率和基质效应均符合染发剂样品测定的要求,用于实际样品测定,结果满意。该方法快速简便、定量准确,能满足染发剂中8种合成染料含量的分析检测要求。     

超高效液相色谱-串联质谱法同时测定染发剂中6种染料

建立了同时测定染发剂中4,4'-二氨基二苯胺硫酸盐和2,4-二氨基苯酚硫酸盐等6种染料的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法.以水为提取剂进行超声提取,用Waters BEH-C₁₈柱(100 mm×2.1 mm, 1.7 μm)分离,以10 mmol/L的乙酸铵和乙腈为流动相进行梯度洗脱.在电喷雾正离子模式下,采用多反应监测(MRM)模式进行定性和定量分析.6种染料在相应的质量浓度范围内线性关系良好,线性相关系数(R²)均大于0.99,检出限为0.26~4.6 mg/kg,回收率为83.0%~92.2%,相对标准偏差为5.4%~11.2%.方法精密度、准确度、回收率和基质效应均符合染发剂样品测定的要求,用于实际样品测定,结果满意.本方法准确、简便、快速,适用于染发剂中6种染料的分析测定.     

超高效液相色谱法同时测定牙膏中5种植物源活性成分

建立了同时测定牙膏中丹皮酚(Pae)、麝香草酚(Thy)、和厚朴酚(Hon)、厚朴酚(Mag)、甘草次酸(Gly)5种植物源活性成分的超高效液相色谱方法。牙膏样品以90%甲醇为溶剂超声提取,离心取上清液过滤后进行分析,采用Waters ACQUITY UPLCHSS C_(18)(2. 1 mm×100 mm,1. 8μm)为分离柱,乙腈-0. 1%甲酸(pH 2. 8)为流动相,梯度洗脱,流速为0. 3 mL/min,二极管阵列检测器(PDA)的检测波长为275、250nm,外标法定量。结果表明,5种植物源活性成分在2～100 mg/L质量浓度范围内呈良好的线性关系,相关系数(r)均大于0. 999;检出限为0. 2～1. 0 mg/kg,定量下限为0. 8～3. 5 mg/kg;在4个加标水平下的平均回收率为90. 5%～99. 4%,相对标准偏差(RSD)为0. 7%～5. 1%。该法分析快速、重复性好、准确性好、灵敏度高,已应用于实际牙膏样品的测定。     

高效液相色谱法测定氧化型染发剂中11种染料

提出了高效液相色谱法测定氧化型染发剂中11种染料含量的方法。样品用甲醇-水(1+1)溶液超声萃取15min,经Capcell Pak C18MG S5色谱柱(250mm×4.6mm,5μm)分离,用磷酸调至pH 7.7的乙腈-三乙胺磷酸缓冲溶液(3+97)为流动相进行等度洗脱,用二极管阵列检测器于波长280nm处检测。11种染料的线性范围均在20～500mg·L-1之间。以空白染发剂样品为基体,进行加标回收试验,回收率在70%～110%之间,相对标准偏差(n=6)均小于10%。     

高效液相色谱法同时测定氧化型染发产品中33种染发剂

建立了高效液相色谱同时测定氧化型染发产品中33种禁限用染发剂含量的分析方法。采用Waters Atlantis^® T3 MV Kit色谱柱（250 mm×4.6 mm，5 μm），以磷酸盐缓冲液-乙腈为流动相，梯度洗脱，流速为1.0 mL/min，柱温为25℃；采用二极管阵列检测器（DAD），检测波长为235及280 nm，进样量为5 μL。结果表明，各成分在线性范围内线性关系良好，相关系数均高于0.999，各成分精密度实验相对标准偏差（RSDs）均小于2%；四氨基嘧啶硫酸盐和2，4-二氨基苯氧基乙醇盐酸盐在12 h内稳定性实验RSDs小于5%，其余31种成分在24 h内稳定性实验RSDs均小于5%；各成分在3个浓度水平下的加标回收率为77.6%~116.3%。该方法简便、快速、准确，适用于氧化型染发产品中多种染发剂的检测。     

高效液相色谱法测定染发剂中的22种染料成分

建立了染发剂中22种染料成分的高效液相色谱测定方法。使用Discovery RP-Amide C16柱(250 mm×4.6 mm,5 μm),以乙腈-0.025 mol/L磷酸盐缓冲液(pH 6.0,含0.1%的庚烷磺酸钠离子对试剂)为流动相,流速为1.0 mL/min;使用二极管阵列检测器(DAD),检测波长为260 nm和280 nm,柱温为25 ℃。该方法除了对低浓度的甲苯-2,5-二胺硫酸盐、2-甲基雷锁辛和N,N-二乙基甲苯-2,5-二胺HCl外,对其他各组分的含量测定值的相对标准偏差(RSD)均小于10%,加标回收率为77.6%～122.8%。该方法简便、准确、快速,适于氧化型染发剂中染料成分的检测。     

高效液相色谱法同时测定染发剂中10种苯二胺衍生物

建立了高效液相色谱法同时测定染发剂中10种苯二胺衍生物的分析方法。采用Discovery RP-Amide C16柱(250×4.6mm,5μm),以25mmol/L磷酸盐缓冲液(pH=6.0,含0.1%的辛烷磺酸钠)和乙腈为流动相,梯度洗脱,流速1.0 mL/min,柱温25℃,检测波长250nm和280nm。各组分的线性范围为0.1~400mg/L,相关系数r为0.9992~0.9999,检出限为18~113mg/kg,定量限为42~373mg/kg,相对标准偏差(RSD)10%,加标回收率为86%~115%。该方法具有简便、快速、准确等特点,基本满足实际样品的分析要求。     

高效液相色谱法同时测定染发剂中11种氨基苯酚

建立了高效液相色谱测定直接型与氧化型染发剂中11种氨基苯酚含量的分析方法。样品在亚硫酸氢钠的保护下用甲醇提取,高速冷冻离心净化;采用Agilent Zorbax SB C18色谱柱分离,流动相为5 mmol/L庚烷磺酸钠-40 mmol/L pH 2.8磷酸盐缓冲液和乙腈,梯度洗脱,11种氨基苯酚分别于230、270和400 nm下检测。11种氨基苯酚在0.05～500 mg/L线性范围内相关系数不小于0.9992,4-氨基-3-硝基苯酚、2-氨基-5-硝基苯酚、3-硝基-4-(2-羟乙基)氨基苯酚的方法定量限为5 mg/kg,其他8种氨基苯酚包括对氨基苯酚、对甲氨基苯酚、间氨基苯酚、邻氨基苯酚、5-氨基-2-甲基苯酚、4-氨基-3-甲基苯酚、2-甲基-5-(2-羟乙基)氨基苯酚和2-氨基-4-硝基苯酚定量限为20 mg/kg,方法回收率为88.5%～109.5%,相对标准偏差为2.2%～8.3%。测定了多种市售染发剂,结果表明该方法操作简单、测定结果准确,可用于直接型与氧化型染发剂中11种氨基苯酚的测定。     

UPLC-MS/MS同时检测染发剂中三种二氨基酚类物质

建立了超高效液相色谱-串联质谱( UPLC-MS/MS)同时检测染发剂中三种二氨基酚类物质(2,4-二氨基苯酚盐酸盐、2,4-二氨基苯甲醚盐酸盐、2,3-二氨基苯酚)含量的方法.样品经0.1％甲酸水溶液提取,正己烷净化后,用Waters ACQUITY BEH Shield RP18色谱柱进行分离,流动相为甲醇和5 m...     

Simultaneous determination of dihydroxybenzenes, aminophenols and phenylenediamines in hair dyes by high-performance liquid chromatography on hypercross-linked polystyrene

The retention of polar organic molecules such as dihydroxybenzenes, aminophenols and phenylenediamines on a 250 x 4.6 mm id column packed with 5 microns hypercross-linked polystyrene Chromalite 5HGN (Purolite) was studied. The influence of separation parameters such as concentration of acetonitrile, buffer (citrate, phosphate) concentration, ionic strength and pH of the eluent on their retention was investigated. Under optimum conditions [acetonitrile-0.3 mol l-1 ammonium phosphate, pH 5.15 (30:70 v/v)], eight substances generally used as dye intermediates in hair colouring compositions could be separated within 20 min. An HPLC method with spectrophotometric detection is proposed for the simultaneous determination of pyrocatechol, resorcinol, hydroquinone, o-, m- and p-aminophenols and p-phenylenediamine in commercial haircolour products. The detection limits of these compounds are in the range 0.05-0.16 microgram ml-1. The suitability of the method is demonstrated by the analysis of three different permanent hair dyes.     

反相液相色谱法同时检测虾仁中合成色素的研究

建立了食品虾仁中合成色素(酸性大红GR、金黄粉、橙黄G、酸性红1号、酸性红26)的反相液相色谱同时检测方法。并且对提取剂、NH4Ac浓度和离子对种类等因素进行优化,使得5种色素完全分离,并且在色谱图上能与国标内的6种色素完全分离。金黄粉、酸性大红GR、橙黄G、酸性红1号、酸性红26的回收率均在80%以上,在0.05~10μg/mL范围内有良好的线性关系,相关系数大于0.9998。本法可用于食品虾仁中合成着色剂的快速检测。     

Simultaneous determination of phenylenediamine isomers and dihydroxybenzene isomers in hair dyes by capillary zone electrophoresis coupled with amperometric detection

The simultaneous determination of three isomers of phenylenediamines (o, m, and p-phenylenediamine) and two isomers of dihydroxybenzenes (catechol and resorcinol) in hair dyes was performed by capillary zone electrophoresis coupled with amperometric detection (CZE–AD). The effects of working electrode potential, pH and concentration of running buffer, separation voltage, and injection time on CZE–AD were investigated. Under the optimum conditions the five analytes could be perfectly separated in 0.30 mol L⁻¹ borate–0.40 mol L⁻¹ phosphate buffer (pH 5.8) within 15 min. A 300 μm diameter platinum electrode had good responses at +0.85 V (versus SCE) for the five analytes. Their linear ranges were from 1.0 × 10⁻⁶ to 1.0 × 10⁻⁴ mol L⁻¹ and the detection limits were as low as 10⁻⁷ mol L⁻¹ (S/N = 3). This working electrode was successfully used to analyze eight kinds of hair dye sample with recoveries in the range 91.0–108.0% and RSDs less than 5.0%. These results demonstrated that capillary zone electrophoresis coupled with electrochemical detection using a platinum working electrode as detector was convenient, highly sensitive, highly repeatable and could be used in the rapid determination of practical samples. Figure Electropherograms obtained from 10 mg mL⁻¹ hair dye sample solutions at a platinum working electrode under optimum CZE–AD conditions: (a) natural black (I), (b) golden: (1) p-phenylenediamine, (2) m-phenylenediamine, (3) o-phenylenediamine, (4) resorcinol, and (5) catechol     

固相萃取-超快速液相色谱-串联质谱法同时测定血液中的4种苏丹染料

建立了血液样品中4种苏丹染料（苏丹Ⅰ、Ⅱ、Ⅲ和Ⅳ）的固相萃取-超快速液相色谱-串联质谱（UFLC-MS/MS）测定方法。样品经乙腈涡旋振荡提取,上清液加等体积水稀释混匀后移入C18固相萃取小柱净化,采用Agilent Eclipse Plus C18色谱柱（100 mm×2.1 mm,1.8 μm）以0.1%（v/v）甲酸水溶液和0.1%（v/v）甲酸乙腈溶液为流动相梯度洗脱分离,电喷雾电离（ESI）正离子多反应监测模式进行定量分析。讨论了苏丹Ⅲ和苏丹Ⅳ的偶氮基团E-Z光学异构现象,并对影响因素进行了分析。结果4种苏丹染料在0.1~20.0 μg/L范围内线性关系良好,相关系数均大于0.999;在低、中、高3个加标水平的平均回收率为93.0%~108.2%,相对标准偏差为4.8%~9.5%;方法的检出限（LOD）为0.06 μg/L,定量限（LOQ）为0.2 μg/L。本方法准确、快速、灵敏,可用于血液样品中苏丹类染料的检测分析。     

HPCE法同时测定蒲公英中的四种组分

建立了高效毛细管电泳(HPCE)同时测定蒲公英中黄酮类化合物、咖啡酸和绿原酸的方法.在优化条件下,4种组分在10min内得到良好分离.绿原酸,异槲皮甙,槲皮素,咖啡酸的线性浓度范围分别为0.003～0.2,0.003～0.2,0.001～0.1,0.001～0.1mg/mL,线性相关系数分别为0.9999、0.9999、0.9998和0.9994.4种组分基于迁移时间和峰高的相对标准偏差分别为0.19%、0.34%、0.20%、0.23%和1.8%、2.6%、2.8%、2.7%.检出限分别为0.56、0.56、0.20和0.21μg/mL.方法可用于中国传统医学中的药物分析.     

气相色谱-质谱法同时测定土壤中的4种丙烯酸酯类农药

建立快速溶剂萃取-气相色谱质谱联用法同时测定土壤中的4种丙烯酸酯类(嘧菌酯,嘧菌胺,苯氧菌胺,醚菌酯)残留量的分析方法。将随机采集到的土壤样品自然风干,粉碎过筛。称取过筛后的样品5 g,置于萃取池中,以丙酮-乙酸乙酯(体积比为1∶1)作为萃取溶剂,于加速溶剂萃取仪中进行提取,收集提取液,氮吹至近干,用丙酮定容至1 mL,以0.45μm滤膜过滤后,上GC-MS/MS仪分析,色谱峰面积外标法定量检测。4种丙烯酸酯类的质量浓度在0.05~5.0μg/mL范围内与其色谱峰面积呈良好的线性关系,检出限为0.006~0.010 mg/kg,加标回收率为91.4%~94.6%,测定结果的相对标准偏差为2.48%~4.29%(n=6)。该方法前处理简单,定性及定量结果准确,适用于土壤中丙烯酸酯类残留的监测。     

Separation and determination of basic dyes formulated in hair care products by capillary electrophoresis

A capillary electrophoretic (CE) method for analyzing five basic dyes (Basic Red 76, Basic Brown 16, Basic Yellow 57, Basic Brown 17 and Basic Blue 99) sold under the trade name Arianor, which are commonly used in hair care products, has been established. A buffer of 100 mM acetic acid-ammonium acetate (50:50) containing 90% (v/v) methanol was employed in a fused-silica capillary of 40.0 cm x 50 microm I.D. with a bubble cell arrangement. Washing the capillary end immediately after injection was effective in preventing peak tailing of the basic dyes, which was due to their adsorption onto the outer wall of the capillary during the injection. Under these optimized conditions, acceptable results for reproducibility, limit of detection and quantitation, and linearity were obtained for the five authentic dyes tested. The recoveries of five authentic basic dyes spiked to three commercial hair care products also provided with acceptable results. This optimized CE method is useful for the analysis of mixed basic dyes in hair care products.