高效液相色谱法测定化妆品中的12种紫外吸收剂

建立了高效液相色谱同时测定化妆品中12种紫外吸收剂含量的方法。样品用甲醇提取,高速离心,过滤,以SB-C8柱(250 mm×4.6 mm, 5 μm)为分离色谱柱,甲醇和0.1%(v/v)甲酸水溶液为流动相,梯度洗脱,以311 nm为检测波长进行定性、定量分析。该方法前处理简单、易操作,12种紫外吸收剂分离效果良好;在1.0～500 mg/L范围内呈线性关系,相关系数大于0.9995;方法检出限为0.002～0.1 mg/L;实际样品中的加标回收率为97.4%～107.5%,相对标准偏差为1.54%～4.98%。该方法简便、准确,能够满足化妆品中紫外吸收剂的检测要求。     

气相色谱法同时测定防晒类化妆品中13种紫外吸收剂北大核心CSCD

采用气相色谱法同时测定防晒类化妆品中13种紫外吸收剂的含量。化妆品样品用甲醇超声提取,用Agilent DB-5色谱柱(30m×0.25mm,0.25μm)分离,氢火焰离子化检测器检测。13种紫外吸收剂的质量浓度均在10.0～500.0mg·L^(-1)内与其对应的峰面积呈线性关系,方法的检出限(3S/N)为2.0～5.0 mg·L^(-1)。以空白样品为基体进行加标回收试验,所得回收率为91.0%～106%,测定值的相对标准偏差(n=6)为0.040%～6.3%。     

高效液相色谱-串联质谱法同时检测化妆品中6种禁用着色剂

建立了高效液相色谱-串联质谱(HPLC-MS/MS)同时测定膏状和粉状化妆品中苏丹红IV、酸性紫49、苏丹蓝2、溶剂红49、碱性紫1和颜料橙5等6种禁用着色剂的检测方法。样品经乙醇-乙腈(3:2, v/v)超声振荡提取20 min、离心净化及氮吹浓缩后,在Luna C18色谱柱(150 mm×2.1 mm, 5 μm)上进行反相液相色谱分离,以甲醇和10 mmol/L乙酸铵溶液为流动相进行梯度洗脱,采用多反应监测(MRM)模式进行质谱测定。根据保留时间及质谱图上特征离子的相对丰度比进行定性,外标法定量。结果表明: 6种着色剂的定量限(信噪比为10计)为0.1～10 μg/kg,回收率为86.67%～98.22%,相对标准偏差(RSD)为4.01%～7.01%。该方法简便、快速、灵敏度高且重现性好,适合于化妆品中禁用着色剂的定性与定量。     

高效液相色谱法测定化妆品中11种二苯酮类紫外线吸收剂

建立了化妆品中11种二苯酮类紫外线吸收剂的高效液相色谱分析方法。采用四氢呋喃-甲醇-水或二氯甲烷-水体系提取化妆品中二苯酮类紫外线吸收剂,经离心(5000 r/min),上清液过0.22 μm滤膜后,进入高效液相色谱分析。采用C18色谱柱进行分离,以0.1% (体积分数)甲酸水溶液(含10 mmol/L乙酸铵)为流动相A,以0.1% (体积分数)甲酸甲醇为流动相B,梯度洗脱。方法加标回收率(n=7)为93.4%~103.8%,相对标准偏差为0.1%~4.2%,方法的检出限为4.0~30 μg/g,方法的定量限为15~100 μg/g。采用该方法对42种市售化妆品检测分析发现,有5种二苯酮类紫外线吸收剂被检出,其中防晒隔离液中二苯酮-3和香水中二苯酮-2的检出量分别为2785 μg/g和2106 μg/g。研究结果表明,所建立的方法具有良好的回收率、重现性和较高的灵敏度,可用于化妆品中多种二苯酮类紫外线吸收剂的分析。     

高效液相色谱法同时测定化妆品中的11种紫外吸收剂

建立了高效液相色谱法准确、快速、灵敏测定化妆品中11种紫外吸收剂的方法。采用C18色谱柱,以乙腈和0.1%甲酸作为流动相,311 nm作为检测波长,在11.5 min内完成11种紫外吸收剂的基线分离。在优化的实验条件下,目标化合物的保留时间和峰面积的相对标准偏差分别小于0.05%和1.20%;另外,所有目标化合物的检出限均低于2.24 mg/L,并在5~500 mg/L内均具有良好的线性关系(R2>0.9990),样品加标回收率为77%~116%。上述结果表明,本方法具有简便、准确、灵敏的特点。对两种不同化妆品中2-羟基-4甲氧基二苯甲酮-5-磺酸、对-氨基苯甲酸等11种紫外吸收剂的测定结果表明,2-羟基-4-甲氧基二苯甲酮、丁基甲氧基二苯酰基甲烷、水杨酸-2-乙基己酯、3,3,5-三甲基环已烷水杨酸酯4种紫外吸收剂在具有防晒功能的化妆品中较为常见,其中3,3,5-三甲基环已烷水杨酸酯在所测化妆品中浓度最高。     

固相萃取-超高效液相色谱-串联质谱法同时测定食品接触塑料制品中10种苯并三唑类紫外吸收剂

建立了固相萃取-超高效液相色谱-串联质谱(SPE-UPLC-MS/MS)同时测定食品接触塑料制品中10种苯并三唑类(BZTs)紫外吸收剂的方法。食品接触塑料制品使用甲醇-二氯甲烷混合溶剂超声提取,C18固相萃取柱净化后用Waters ACQUITY UPLC BEH C₁₈色谱柱(100 mm×2.1 mm, 1.7 μm)分离,甲醇和0.1%(v/v)甲酸水溶液为流动相进行梯度洗脱,多反应监测(MRM)模式检测,外标法定量分析。结果表明,10种BZTs在线性范围内线性关系良好,线性相关系数(r²)均大于0.996;检出限为0.6~1.6 μg/kg; 3个水平下的加标回收率为75.2%~85.3%,相对标准偏差为1.0%~5.7%。该方法准确、简便、快速、检出限低,可用于食品接触塑料制品中10种BZTs的同时检测。     

高效液相色谱法同时测定防晒类化妆品中15种紫外线吸收剂

建立了一种反相高效液相色谱同时测定防晒类化妆品中15种紫外线吸收剂的分析方法。化妆水、乳液、膏霜和蜡质样品中首先加入四氢呋喃(含2 g/L氢氧化铵),涡旋、振荡、混匀(若蜡质样品仍分散不完全,可超声振荡加热至50 ℃),再加入80%(v/v)甲醇水溶液振荡混匀、超声提取、离心、过滤后,采用XTerra MS C₁₈柱分离,经水(含0.1%(v/v)甲酸)和甲醇(含0.1%(v/v)甲酸)梯度洗脱,以二极管阵列检测器检测,检测波长为280 nm和311 nm,外标法定量。实验中对不同基质类型样品的前处理条件(样品分散溶剂、萃取溶剂和萃取时间等)进行了重点优化。结果表明,15种紫外线吸收剂在各自的线性范围内呈良好的线性关系(r²≥0.9991),方法的定量限为1.2~5.1 μg/g,在低、中、高3个添加水平下的回收率为84.2%~100.7%,相对标准偏差(RSD)为0.9%~9.5%。该分析方法分离效果好、灵敏度高、定量准确,可用于防晒类化妆品的实际检测。     

高效液相色谱-串联质谱法测定化妆品中的欧前胡素和异欧前胡素

建立了化妆品中欧前胡素和异欧前胡素的高效液相色谱-串联质谱(HPLC-MS/MS)测定与确证方法。样品经甲醇提取,以C18柱为分离柱,10 mmol/L乙酸铵/甲醇溶液-5 mmol/L乙酸铵水溶液(80:20, v/v)为流动相分离,采用电喷雾串联四极杆质谱进行检测。欧前胡素和异欧前胡素在0.25～20 μg/L内线性良好(相关系数大于0.999);方法定量限(LOQ)为0.50 mg/kg。在0.50～10.0 mg/kg内,欧前胡素和异欧前胡素的回收率范围分别为82.2%～105%和80.0%～103%,相对标准偏差分别为2.7%～4.9%和1.8%～4.6%。该方法能够满足化妆品中欧前胡素和异欧前胡素检测的需要。     

超高效液相色谱法测定涂料中11种紫外吸收剂

建立了同时测定涂料中11种苯甲酮类和苯并三唑类紫外吸收剂的超高效液相色谱(UPLC)分析方法。乳胶漆类样品经水分散后,乙酸乙酯提取;木器清漆类样品以乙腈直接提取。提取液以C18色谱柱为分离柱,在乙腈-水流动相体系下变流速洗脱分离,二极管阵列检测器检测。结果表明,11种紫外吸收剂在0.1~50 mg/L浓度范围内线性关系良好,相关系数(r)均不小于0.999 0;方法检出限为10~30 mg/kg;3个加标水平下的平均回收率(n=6)为80.7%~107%,相对标准偏差(RSD)为3.0%~8.7%。该方法简单、快速,回收率和精密度良好,适用于涂料中11种紫外吸收剂的同时测定。     

高效液相色谱-串联质谱法测定食品中6种人工合成甜味剂

建立了食品中6种人工合成甜味剂(甜蜜素、糖精钠、安赛蜜、阿斯巴甜、阿力甜、纽甜)的高效液相色谱-串联质谱检测方法。样品经甲醇-水溶液(1:1, v/v)提取,以C18柱为分离柱,0.1%(v/v)甲酸-5 mmol/L甲酸铵溶液/乙腈为流动相,经高效液相色谱分离,采用电喷雾串联四极杆质谱进行检测。结果表明,6种人工合成甜味剂在20～500 μg/L范围内定量离子对的响应峰面积和样品质量浓度之间有良好的线性关系(相关系数＞0.998)。在3个添加水平下,样品平均回收率为81.3%～106.0%,相对标准偏差小于11%。该方法简单、灵敏、准确,可用于食品中6种人工合成甜味剂的同时检测。     

高效液相色谱法同时测定食品接触材料中抗氧化剂和紫外吸收剂的迁移量

采用高效液相色谱技术,建立了食品接触材料中多种抗氧化剂和紫外吸收剂迁移水平的检测方法。该方法测定的23种目标化合物具有较好的线性关系,相关系数（r²）≥ 0.9998,检出限和定量限分别在0.01到0.22 mg/L之间和0.03到0.85 mg/L之间。依据欧盟指令（EU）No. 10/2011,考察了5种食品模拟物30 g/L乙酸、10%（v/v）乙醇、20%（v/v）乙醇、50%（v/v）乙醇和油类模拟物（异辛烷）中抗氧化剂和紫外吸收剂的迁移量。该方法回收率在92.8%~117.7%之间,相对标准偏差在0.95%~9.72%之间。探讨了不同实验条件对抗氧化剂和紫外吸收剂回收率的影响。结果表明,该方法准确、稳定,完全满足欧盟指令（EU）No 10/2011和GB 9685-2008对食品接触材料及制品中抗氧化剂和紫外吸收剂特定迁移量（SML）的限量要求,并利用该方法测定了30批次食品接触材料中抗氧化剂和紫外吸收剂的迁移水平。     

高效液相色谱-串联质谱法测定化妆品中10种生物碱

建立高效液相色谱-串联质谱同时测定化妆中10种生物碱的分析方法。实验优化了提取条件、净化方式和仪器条件等参数。样品经80%（v/v）甲醇水溶液超声提取，离心后过滤。采用Waters BEH C₁₈色谱柱分离，在多反应监测模式下测定，外标法定量。结果显示，在各自范围内，10种生物碱具有良好的线性关系，相关系数（R²）>0.9900，方法的检出限为5.0~12.5 μg/kg，定量限为12.5~50.0 μg/kg。在1倍、2倍和6倍定量限的加标水平下，10种生物碱的回收率为70.91%~116.75%，相对标准偏差为0.49%~9.98%（n=6）。该方法操作简单，适用于化妆品中10种有毒生物碱的快速筛查和定量分析。     

气相色谱-质谱法测定化妆品中的防晒剂

采用气相色谱-质谱法测定了化妆品中11种防晒剂，通过对提取溶剂、提取条件的选择和线性、灵敏度、精密度、回收率等的研究，建立了测定化妆品中防晒剂的方法，11种防晒剂的平均回收率(n＝5)在98．2％-101．2％之间，相对标准偏差(n＝5)在0．3％-1．6％之间。     

Development and validation of UPLC‐MS/MS method for determination of domperidone in human plasma and its pharmacokinetic application

A sensitive, rapid and selective ultra‐performance liquid chromatography–tandem mass spectrometric (UPLC‐MS/MS) method was developed for the determination and pharmacokinetic study of domperidone in human plasma. Diphenhydramine was used as the internal standard. Plasma sample pretreatment involved a one‐step liquid–liquid extraction with a mixture of diethyl ether–dichloromethane (3:2, v/v). The analysis was carried out on an Acquity UPLC^TM BEH C₁₈ column. The mobile phase consisted of methanol–water containing 10 mmol/L ammonium acetate and 0.5% (v/v) formic acid (60:40, v/v). The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring mode via electrospray ionizationsource with positive mode. Each plasma sample was chromatographed within 2.1 min. The standard curves for domperidone were linear (r² ≥ 0.99) over the concentration range of 0.030–31.5 ng/mL with a lower limit of quantification of 0.030 ng/mL. The intra‐ and inter‐day precision (relative standard deviation) values were not higher than 13% and accuracy (relative error) was from ?7.6 to 1.2% at three quality control levels. The method herein described was superior to previous methods and was successfully applied to the pharmacokinetic study of domperidone in healthy Chinese volunteers after oral administration. Copyright © 2012 John Wiley & Sons, Ltd.     

Determination of pseudo‐ginsenoside GQ in human plasma by high performance liquid chromatography–tandem mass spectrometry

A specific, sensitive and rapid method based on high performance liquid chromatography coupled to tandem mass spectrometry (HPLC‐MS/MS) was developed for the determination of pseudo‐ginsenoside GQ in human plasma. Liquid–liquid extraction was used to isolate the analyte from biological matrix followed by injection of the extracts onto a C₈ column with isocratic elution. Detection was carried out on a triple quadrupole tandem mass spectrometer (API‐4000 system) in multiple reaction monitoring mode using negative electrospray ionization. The mobile phase consisted of methanol–10 mm ammonium acetate (90:10, v/v) and the flow rate was 0.3 mL/min. The method was validated over the concentration range of 5.0–5000.0 ng/mL for plasma. Inter‐ and intra‐day precisions (relative standard deviation) were all within 15% and the accuracy (relative error) was ≤9.4%. The lower limit of quantitation was 5.0 ng/mL. The pseudo‐ginsenoside GQ was stable after 8 h at room temperature, 24 h at autosampler and three freeze–thaw cycles (from ?30 to 25 °C). The method was successfully applied to the pharmacokinetic study of pseudo‐ginsenoside GQ in healthy Chinese volunteers. Copyright © 2013 John Wiley & Sons, Ltd.     

A novel UPLC‐MS/MS method for sensitive quantitation of boldine in plasma,a potential anti‐inflammatory agent: application to a pharmacokinetic study in rats

Boldine is a potential anti‐inflammatory agent found in several different plants. Published bioanalytical methods using HPLC with ultraviolet and fluorescent detection lacked enough sensitivity and required tedious sample preparation procedures. Herein, we describe the development of a novel ultra‐high performance LC with MS/MS for determination of boldine in plasma. Boldine in plasma was recovered by liquid–liquid extraction using 1 mL of methyl tert‐butyl ether. Chromatographic separation was performed on a C₁₈ column at 45°C, with a gradient elution consisting of acetonitrile and water containing 0.1% (v/v) formic acid at a flow rate of 0.3 mL/min. The detection was performed on an electrospray triple‐quadrupole MS/MS by positive ion multiple reaction monitoring mode. Good linearity (r² > 0.9926) was achieved in a concentration range of 2.555–2555 ng/mL with a lower limit of quantification of 2.555 ng/mL for boldine. The intra‐ and inter‐day precisions of the assay were 1.2–6.0 and 1.8–7.4% relative standard deviation with an accuracy of ?6.0–8.0% relative error. This newly developed method was successfully applied to a single low‐dose pharmacokinetic study in rats and was demonstrated to be simpler and more sensitive than the published methods, allowing boldine quantification in reduced plasma volume. Copyright © 2014 John Wiley & Sons, Ltd.     

Analysis of Morpholinium Ionic Liquid Cations by Hydrophilic Interaction Columns Coupled with Indirect UV Detection

A method was developed for the separation and detection of morpholinium ionic liquid cations by hydrophilic interaction column combined with indirect ultraviolet detection using imidazolium ionic liquids as ultraviolet absorbents in high‐performance liquid chromatography. The effects of the ultraviolet absorbents, organic solvents, and the pH value of the aqueous solution in the mobile phase for the determination of morpholinium cations were investigated by using a hydrophilic column with carbamoyl group as the analytical column. The retention and detection behavior of morpholinium cations was discussed. The suitable chromatographic conditions were 0.8 mmol/L 1‐ethyl‐3‐methyl‐imidazolium tetrafluoroborate aqueous solution (pH 3.5 adjusted with acetic acid)/acetonitrile (45/55, v/v) as the mobile phase and a detection wavelength of 210 nm. Under these conditions, the baseline separation of N‐methyl‐N‐ethyl‐morpholinium cation ([MEMo]⁺) and N‐methyl‐N‐propyl‐morpholinium cation ([MPMo]⁺) was successfully achieved in 15 min. The detection limits of [MEMo]⁺ and [MPMo]⁺ were 0.595 and 0.531 mg/L, respectively. Relative standard deviations were less than 0.2%. This method has been successfully applied to the analysis of morpholinium ionic liquid samples synthesized in chemical laboratories, which is simple, reliable, and practical.