HPLC-MS联用测定果冻等食品中的3种甜味剂和苯甲酸

建立食品中糖精钠、甜蜜素、安赛蜜和苯甲酸的高效液相色谱-质谱（HPLC-MS）检测方法。色谱柱为Spherigel C18（5μm,4．6×200Mm）,流动相为：（A）甲醇-（B）甲酸-三乙胺缓冲盐,梯度洗脱;电喷雾负离子（ESI^-）采集模式,流速为1．0mL／min,进样量为10μL;以华法林钠为内标,质谱定性定量;安赛蜜、糖精钠、甜蜜素、苯甲酸的线性范围分别为：5．4～135,5．4～135,7．4～111,10～150μg／mL,加样回收率为93．19％～100．90％,RSD为1．05％～2．04％．该方法具有选择性好、分析时间短、定性定量准确等优点,可用于果冻等食品中的4种目标物定性定量检测。     

UPLC-MS/MS快速筛查豆芽中27 种植物生长调节剂和抗生素类药物

目的：建立超高效液相色谱-串联质谱快速筛查豆芽中27 种植物生长调节剂和抗生素类药物的方法。方法：采用Agilent Eclipse Plus-C18（2.1 mm×100 mm，1.8 μm）色谱柱，以0.01%甲酸为流动相A，甲醇为流动相B，梯度洗脱，流速为0.4 mL/min，质谱选择多反应监测模式对27 种植物生长调节剂和抗生素类药物进行定性和定量检测。结果：该方法线性范围宽、相关性好，R2≥0.998 5；精密度相对标准偏差为1.1%～3.5%（n=6）；方法采用3 个添加水平进行加样回收实验，回收率范围为80.5%～114.9%；检出限为0.5～50 μg/kg，定量限为1.5～150 μg/kg。结论：该方法快速、专属性强、灵敏度高，可同时完成豆芽中27 种植物生长调节剂和抗生素类药物的检测。     

超高效液相色谱-串联质谱法检测植物源加工食品中农药残留

目的 建立植物源性预包装食品中35种农药残留的超高效液相色谱-串联质谱检测方法。方法 样品经乙腈提取,QuEChERS方法净化,经Shim-pack GIST C18色谱柱分离,以乙腈和0.1％甲酸水溶液为流动相进行梯度洗脱,电喷雾正离子(ESI+)/负离子(ESI-)模式电离,MRM扫描模式检测。结果 经方法学验证,本方法的线性关系、回收率、精密度均符合要求。结论 可实现植物源性预包装食品中35种农药残留的同时定性、定量分析。本方法重现性好,回收率高。     

食品中虾青素的C18-HPLC-PDA分离与鉴定

在装备了二极管阵列检测器(PDA)的高压液相色谱(HPLC)上,应用C18柱,冰凉花和虾中的主要酮基类胡萝卜素-虾青素可以被分离。分离条件为:色谱柱为DiamonsilTM(5μm,4.6mm×25cm,DikmaTechnology);流动相A为乙腈-水(90∶10,V/V),用磷酸调pH3.0;流动相B为乙酸乙酯;线性梯度洗脱:B在15min内由0%增加至70%;15～25min内B维持在70%;流速=1.0mL/min;检测波长=480nm;PDA波长范围=280～580nm;进样量=20mL。根据其与参比样品的色谱行为和光谱特征比较,样品中的虾青素可被鉴定。它在C18-HPLC-PDA上的定量亦成为可能。     

番茄和胡萝卜中类胡萝卜素的C30与C18HPLC分离

为提高胡萝卜素的分离水平,在相同的HPLC条件下比较了C30与C18柱对番茄和胡萝卜中类胡萝卜素的分离情况.比较的色谱条件为C30固定相YMCTM Carotenoid S-5柱(YMC,250 mm×4.6 mm,5μl);C18固定相DIAMONSILTM柱(Dikma Technologies,250 mm×4.6 mm,5 μl);流动相A乙腈+水=9+1;流动相B乙酸乙酯;线性梯度洗脱在前15 min内,B由0%增为100%,随后,B保持100%,流速为1.0 ml/min,检测波长为450 nm,进样量为20μl,室温.从二者色谱图的比较可以看出,C30柱反相高效液相色谱在分离几何异构体上显示出明显的优势,可有效分离成分复杂、多样、结构相似的不合氧类胡萝卜素顺反异构体.可以认为,C30柱在分析食品中类胡萝卜素组分的领域中具有良好的应用前景.     

超高压液相色谱-电喷雾串联四极杆质谱法测定猪肉食品中8种β-受体激动剂

目的 采用超高压液相色谱-电喷雾串连四极杆质谱同时测定猪肉食品中8种β-受体激动剂残留。方法 试样中β-受体激动剂残留经酶解后超声提取, 低温离心后, 上清液用MCX固相萃取柱净化, Waters ACQUITY UPLCTM BEH C18色谱柱分离, 以甲醇?0.1%甲酸水溶液为流动相梯度洗脱, 最后用液相色谱-质谱/质谱进行测定。结果 该方法的平均回收率为75.6%~118.7%, 相对标准偏差小于25.0%, 方法的定量限为0.1~0.2 μg/kg。结论 该方法操作简单, 灵敏度高, 重现性良好, 适用于猪肉食品中β-受体激动剂残留的定性与定量检测。     

高效液相色谱-串联质谱法同时测定食品中9种人工色素

目的建立一种同时测定食品中9种人工色素(赤藓红、诱惑红、柠檬黄、亮蓝、靛蓝、胭脂红、苋菜红、日落黄、新红)的高效液相色谱-串联质谱(high performance liquid chromatography-tandem mass spectrometry,HPLC-MS/MS)检测方法。方法 3种食品样品分别经3种不同的固相萃取柱净化方法净化,采用甲醇(A)和10 mmol/L乙酸铵(B)为流动相,梯度洗脱分离,电喷雾离子化,正离子扫描,多反应监测对9种人工色素进行定性和定量。结果本方法在15 min内完成9种目标化合物的分离分析;采用PLS固相萃取小柱进行前处理,各色素在100μg/kg添加水平的回收率为98.1%~102.3%,结论该前处理方法回收率高,仪器方法快速、准确、灵敏,适合测定食品中9种人工色素。     

酱腌菜中三氯蔗糖的检测

实验利用液相色谱质谱联用的检测方法(LV-MS)进行检测,样品经水超声提取,亚铁氰化钾和乙酸锌溶液去除蛋白等杂质后,用甲醇和水作为流动相进行梯度洗脱,资生堂MGⅡC₁₈色谱柱(5 μm,100 mm×2.1 mm)分离,电喷雾负离子模式电离,以395/359为定量离子,395/36为定性离子,进行定性定量分析,方法定量限为0.5mg/kg。     

真丝织物上茶多酚的高效液相色谱法检测

为建立真丝织物上茶多酚的高效液相色谱检测方法,探讨了检测波长、流动相洗脱程序、样品进样体积、流动相流速和色谱柱柱体温度对检测方法的影响。得到色谱条件:采用Red Classical C18色谱柱,检测波长278 nm、进样体积10μL、柱温35℃、流动相流速1 000μL/min,在优化的流动相系统洗脱程序下梯度洗脱。得到了茶多酚中3种主要成分、茶多酚标准品以及织物剥离茶多酚的高效液相色谱图,主要成分峰保留时间基本一致,可对染色织物上剥离的茶多酚进行定性检测。     

利胆颗粒质量标准的研究

目的建立利胆颗粒质量标准。方法薄层色谱法鉴别白芍和姜黄;高效液相色谱法检测橙皮苷含量,色谱柱为Shimadzu VP-ODS C_(18) (250 mm×4.6 mm,5μm);流动相:以乙腈为流动相A,0.2%磷酸溶液为流动相B,梯度洗脱;流速:1.0 ml/min;柱温:30℃;检测波长:283 nm。结果薄层鉴别的色谱斑点清晰,阴性对照无干扰;橙皮苷在19.98～199.8μg/ml范围内呈良好的线性关系(r=0.9999),平均回收率97.41%,RSD为1.696%。结论该测定方法简单可行,可用于利胆颗粒定性、定量检测,可用于利胆颗粒的质量控制。     

反相高效液相色谱法测定烟草中的类胡萝卜素及其异构体

采用反相高效液相色谱−二极管阵列检测器（RP−HPLC−DAD）分离和测定烟草中类胡萝卜素及其异构体的组成和含量。烟草样品经过含有0.1%丁基羟基甲苯（BHT）的冰丙酮溶液萃取,浓缩后,经Zorbax SB C18色谱柱分离。流动相组成:A,乙腈−水（体积比为88:12）;B,乙酸乙酯。梯度洗脱程序:0 − 25min,100%A;25 − 50 min,B由0%线性增加为60%;50 − 55 min, 40%A+ 60% B;55 − 60 min,A由40%线性增加为100%。 检测波长:450 nm。进样量:10 µL。流速:1.0 mL/min。该方法简化了样品的前处理,共分离出烟草中11种类胡萝卜素及其异构体。类胡萝卜素物质的加标回收率为87.7−94.6%,;相对标准偏差为3.01−4.29%。同时研究了新鲜烟叶和烘烤后烟叶中类胡萝卜素的分布和含量,结果显示:烟叶中类胡萝卜素的组成及含量与烟叶品种、部位以及调制有关。      

Validation of a HPLC method for simultaneous determination of five sunscreens in lotion preparation

The aim of this research was to develop and validate a high-performance liquid chromatographic (HPLC) method for simultaneous determination of five sunscreens, namely benzophenone-3 (B-3), butyl methoxydibenzoylmethane (BM), octyl methoxycinnamate (OM), octyl salicylate (OS) and homosalate (HS). The separation and quantitative determination was made by HPLC at 40 +/-1 degrees C with a gradient elution from 10% to 100% mobile phase B in mobile phase A. The gradient liquid chromatographic system constituted of mobile phase A [acetonitrile : water (10 : 90 v/v)] and mobile phase B [acetonitrile : water (90 : 10 v/v)], at a flow rate of 1.0 mL min(-1) and ultraviolet detection at 310 nm. The separation was obtained with two Waters reversed phase columns: Novapack C-18 and Symmetry((R)) C-18 connected in series. All sunscreens were efficiently separated within 17 min. The coefficient of correlation and average recovery for B-3, BM, OM, OS and HS were 0.9798 and 98.5%, 0.9672 and 98.8%, 0.9922 and 99.1%, 0.9961 and 98.9% and 0.9909 and 99.4% respectively. The relative standard deviations obtained were between 1.07% and 2.44%. The excipients did not interfere in the analysis. The results showed that the proposed method could be used for rapid and simultaneous determination of B-3, BM, OM, OS and HS in sunscreen lotions with precision, accuracy and specificity.     

Simultaneous of illegal additives in dietary supplements and traditional medicines by high performance liquid chromatography–electrospray ionization mass spectrometry

A high performance liquid chromatographic method coupling with electrospray ionization mass spectrometry (HPLC/ESI-MS) for simultaneous determination of phenformin, rosiglitazone, glibenclamide and glimepiride in dietary supplements and traditional Chinese medicines for diabetes mellitus was proposed. The separation was achieved on a C₁₈ column with the mobile phase consisted of acetonitrile and water (0.05% formic acid (v/v) and 20 mM ammonium acetate), at a flow rate of 1.0 ml/min with gradient elution. The analytes were identified and quantified by ESI-MS. Sildenafil was selected as internal standard. Full validation of the proposed method was provided (selectivity, linearity, limit of detection, limit of quantification, precision and accuracy). In contrast to existing methods, the proposed method has obvious advantages of simplicity, rapidity, accuracy and good applicability, and it has been applied to analyze illegal additives in nine dietary supplements and eight traditional Chinese medicines successfully.     

反相C30柱在HPLC分析类胡萝卜素中的应用

本文介绍了一种最近在类胡萝卜素高压液相色谱分析中非常引人注目的固定相-反相C30梓，并例举了这种柱子在食品-特别在植物食品-的类胡萝卜素分析中的一些应用实例。与反相C30同定相相比，C30同定相分离类胡萝卜素的几何异构体具有明显的优势。因此，可以认为：应用反相C30柱分析生物样品-特别是食品材料-中的类胡箩卜素会具有良好的前景。     

Determination of bisphenol A in canned vegetables and fruit by high performance liquid chromatography

A high performance liquid chromatograph y (HPLC) method was developed for the determination of bisphenol A (BPA) that had migrated into canned fruit and vegetables. BPA was extracted with acetonitrile from the solid portion of canned food, and with an OASIS HLB cartridge from the aqueous portion, respectively. Both extracts were cleaned up on a Florisil cartridge. The HPLC separation was carried out on a Wakosil II 3C18 RS column (4.6 × 150mm) with acetonitrile-water (40:60, v/v) as a mobile phase with a flow rate of 0.8 ml/min. BPA was detectable by UV detector at 228 nm and determined with the similarity of chromatographic peak spectrum by multiwavelength detector (similarity index was 0.99 or above). The quantification limits were 10 ng/g for the solid portion and 5 ng/ml for the aqueous portion, respectively. BPA was mainly detected in the solid portion of canned food and found at the maximum level of 11 μg per can. To verify migration into the solid portion of canned food, a partitioning experiment was carried out.     

液相色谱-质谱测定饮用水中的溴酸盐和高氯酸盐

建立液相色谱分离、电喷雾四极杆质谱测定饮用水中溴酸盐和高氯酸盐的方法。使用XterraTM C18 色谱柱,以乙腈- 四丁基氢氧化铵溶液为流动相分离,选择离子检测。溴酸盐和高氯酸盐的线性范围均为1.0～200.0ng/mL,方法检出限均为1.0ng/mL。     

A rapid high-performance liquid chromatography with fluorescence detection method developed to analyze ochratoxin A in wine

A rapid, sensitive, reproducible, and inexpensive method of high-performance liquid chromatography with fluorescence detection (HPLC-FLD) for the analysis of ochratoxin A (OTA) in wine was developed. It is characterized by direct injection of the wine into the HPLC apparatus, with no need of extraction or cleanup. The method uses acetonitrile, water, and acetic acid (49:49:2, vol/vol/vol, respectively) as the isocratic mobile phase and a 5-microm monolithic C18 column (100 by 3 mm inside diameter). The relative standard deviation obtained in the OTA determination varied between 0.22 and 1.76%, with a mean value of 0.89%, in samples with concentrations between 0.10 and 100 ng/ml. The recovery of OTA ranged from 102% in samples spiked with 1 ng/ml OTA to 120% in samples with 0.10 ng/ml OTA. The method compared favorably with a published method based on an immunoaffinity column cleanup and a chromatographic assay with a C18 conventional HPLC column.     

HPLC Determination of Sugars and Starch in Green Beans

A reversed-phase HPLC method using a Spherisorb NH₂ column and 85:15 v/v acetonitrile/water as mobile phase was developed for determination of starch and soluble sugars (glucose, fructose and sucrose) in plants. When applied to pure starch samples, the analytical method was as accurate as the official AOAC method and had better precision (coefficient of variation 0.87% vs 1.27%). When applied to green bean (Phaseolus vulgaris L.), recovery was 97.7% for starch, 98.0% for glucose and 98.1% for both fructose and sucrose.     

HPLC method for determining ethylenediamine migration from epoxy-amine food packaging coatings into EU food simulants.

A simple, rapid, sensitive and inexpensive method has been developed for the determination of ethylenediamine (EDA) in European Union food simulants. The method involves precolumn derivatization with ortho-phthaldehyde (OPA) and 2-mercaptoethanol (ME) to obtain a fluorescent derivative. Liquid chromatographic (HPLC) elution was achieved with methanol-ultrapure water (65:35) as mobile phase with a Waters Spherisorb 5 microm ODS 2 column. Fluorescence detection (FD) was performed at 330 nm (excitation wavelength) and 450 nm (emission). Total chromatographic analysis time was < 10 min. The proposed method was validated by checking linearity, detection and quantification limits, and precision. Relative recovery rates were of about 100% because samples and standard-spiked blanks were processed in the same way. Method precision (RSD < 6%) was satisfactory and the quantification limit (0.25 mg x (-1)) indicated that specific migration limit for EDA in EU food simulants (12 mg x kg(-1)) can be easily controlled. When the validated method was applied to epoxy-amine formulations used for can coatings under different curing conditions, EDA migration was < 1.4 mg x l(-1).     

高效液相色谱法同时测定食品中的12种抗氧化剂

目的：建立一种快速、准确测定食品中12 种抗氧化剂的高效液相色谱法。方法：样品用正己烷溶解,用含抗坏血酸棕榈酸盐(AP)的饱和乙腈萃取,以反相C18 柱为分离柱,以甲醇- 乙腈- 乙酸- 水体系为流动相进行梯度洗脱,采用高效液相色谱- 紫外检测器于280nm 定量检测。结果：12 种抗氧化剂在36min 内完全分离,线性范围为0.2～200mg/L(r=0.9981～0.9999),定量限为0.2～1.0mg/kg,回收率为81.13%～107.57%,相对标准偏差为0.26%～4.52%(n=7)。结论：本方法准确、可靠、简便、检出限低,适合分析大批量样品。