超高效液相色谱法测定皮肤科外用药辛伐他汀乳膏中辛伐他汀含量

目的 建立测定辛伐他汀乳膏中辛伐他汀含量的超高效液相色谱(UPLC)法。方法 色谱柱为ACQUITY UPLC BEH C₁₈柱(100 mm×2.1 mm,1.7μm)，流动相为乙腈-水(52∶48,V/V)，流速为0.6 mL/min，检测波长为238 nm，柱温为30℃，进样量为5μL。结果 辛伐他汀质量浓度在4.132～20.660μg/mL范围内与峰面积线性关系良好(R²=0.999 4,n=5)；精密度、稳定性、重复性试验结果的RSD均小于2.0%；平均回收率为100.20%,RSD为2.20%(n=9)。结论 所建立的方法快速，结果准确，可用于辛伐他汀乳膏的质量控制。     

高效液相色谱法测定辛伐他汀滴丸中辛伐他汀的含量

目的建立高效液相色谱法测定辛伐他汀滴丸中辛伐他汀含量的方法。方法以Hypersil ODS(4.6mm×250 mm,5μm)为色谱柱,流动相为乙腈-0.01 mol.L-1磷酸溶液(90∶10),检测波长238 nm,流速1.0mL.m in-1。结果辛伐他汀的线性范围为64.14~384.80μg.mL-1(r=0.999 6),平均回收率为100.20%,RSD=2.90%。日内精密度的RSD为0.13%;日间精密度的RSD为0.38%。结论该方法灵敏、准确、专属性强,可作为辛伐他汀滴丸质量控制的方法。     

高效液相色谱法测定辛伐他汀含量及其有关物质

目的 建立辛伐他汀的含量及其有关物质的高效液相色谱测定方法.方法 色谱柱:Luna C18 (250 mm×4.6 mm,5 μm);流动相:0.025 mol/L 磷酸二氢钠溶液(pH值为4.5):乙腈(35:65);流速:1.0ml/min;检测波长:238 nm;柱温:室温.进样量为20μl.结果 在所选定的液相色谱条件下,有关物质与主药分离良好.回归方程Y=3.256C×103+4.510×102,在2～200 μg/ml 范围内呈现良好的线性(r=0.9996).平均回收率为99.32%,RSD为0.31%(n=9).结论 此方法重现性好,准确度高,专属性强.适用于辛伐他汀的含量测定及相关物质检查.     

高效液相色谱法测定辛伐他汀分散片的含量及其有关物质

目的：采用高效液相色谱法测定辛伐他汀分散片中辛伐他汀及其有关物质的含量。方法：色谱柱ODS-C18柱（250mm×4．6mm，5μm）；以乙腈-0．025mol·L^-1磷酸二氢钠溶液（pH4．5）（65：35）为流动相；检测波长为238nm。结果：回归方程A=48504．5C-31．57，线性范围为1．108×10^-3～1．772×10^-1g·L^-1（r=0．9996），含量测定的平均回收率为99．14％，RSD为0．37％（n=9）。结论：方法重现性好，准确度高，适于辛伐他汀片剂的质量控制。     

超高效液相色谱法测定大豆异黄酮胶囊中异黄酮的含量

目的建立同时测定大豆异黄酮胶囊中6种异黄酮含量的超高效液相色谱法(HPLC)。方法采用AcquityUPLCTMBEHC18柱(1.7μm,2.1mm×50mm),流动相为甲醇-0.05mol/L乙酸胺(pH4.6),梯度洗脱,检测波长为260nm,流速为0.4ml/min,柱温为40℃,外标法测定。结果大豆苷、黄豆黄苷、染料木苷、大豆苷元、黄豆黄素和染料木素分别在0.02600～0.2600mg/ml、0.02625～0.2625mg/ml、0.02675～0.2675mg/ml、0.012650～0.12650mg/ml、0.012525～0.12525mg/ml、0.012750～0.12750mg/ml范围内线性关系良好(r≥0.9930),加样回收率(6例)分别为:98.5%、98.8%、98.2%、97.7%、98.0%、97.3%。结论本法快速、简便、准确、灵敏度高、成本低,适用于大豆异黄酮胶囊中异黄酮的含量测定及质量控制。     

高效液相色谱法测定头孢氨苄胶囊含量

目的：介绍一种用反相高效液相色谱法测定头孢氨苄胶囊含量的方法。方法：以ＳｈｉｍｐａｃｋＣＬＣＯＤＳ（１５０ｍｍ×６ｍｍ,１０μｍ）为色谱柱,甲醇水（７０∶３０）为流动相,检测波长为２６２ｎｍ,外标法定量。结果：头孢氨苄浓度线性范围为１００～９００μｇ·ｍｌ－１,相关系数ｒ＝０．９９９９,方法回收率为９９．７％,ＲＳＤ为０．８９％。结论：方法简便快速,结果准确可靠,可作为头孢氨苄制剂的质量控制方法。     

超高效液相色谱法测定紫参胶囊中芍药苷含量

目的建立超高效液相色谱法测定紫参胶囊中芍药苷含量的方法。方法采用超高效液相色谱法,色谱柱为WatersAcquity BEH C1(82.1 mm×50 mm,1.7μm),流动相为乙腈-0.1%磷酸溶液(15∶85),流速0.25 ml/min,检测波长230 nm,柱温30℃。结果芍药苷在14～84μg/ml范围内与峰面积线性关系良好,r=0.9997,平均加样回收率为97.3%,RSD=1.93%(n=6)。结论本法准确、简便、重现性好,可用于紫参胶囊中芍药苷的含量测定。     

超高效液相色谱法测定烟酸片的含量

目的 建立超高效液相色谱法测定烟酸片的含量的方法.方法 采用高效液相色谱法,色谱条件：waters ACQUITY UPLC HSS T3（2.1×100mm,1.8μm）色谱柱;流动相为甲醇-0.2%冰醋酸溶液（20：80）;检测波长：262nm;流速：0.3mL·min-1.结果 烟酸在5.045～252.3mg·L-1的浓度范围内与峰面积呈良好的线性关系（r=1）,最低检出限为0.026μg·mL-1,平均回收率分别为100.0%;RSD分别为0.2%.结论 本方法专属性好,准确,灵敏,适用于烟酸片的含量测定,结果可靠.     

高效液相色谱法测定罗红霉素胶囊的含量

目的 　建立高效液相色谱法测定罗红霉素胶囊的含量。 方法 　采用 Hypersil ODS C1 8色谱柱 ( 2 5 0 mm× 4.6mm,5 μm) ,以 0 .1mol·L- 1磷酸二氢铵溶液 (三乙胺调节 p H至 6.5 ) -乙腈 ( 2∶ 1)为流动相 ,流速为 1.0 ml· min- 1 ,检测波长为 2 10 nm。结果 　在进样量 5 .0μg～ 80 .0μg的范围内 ,峰面积与进样量之间呈良好的线性关系 ( r=1.0 0 0 0 )。加样回收率为 99.3 6% ,RSD为 0 .87%。 结论 　该方法快速 ,简便 ,重现性好。     

高效液相色谱法测定感冒灵胶囊中4种组分的含量

感冒灵胶囊是由对乙酰氨基酚、咖啡因、盐酸苯丙醇胺 (ＰＰＡ)、马来酸氯苯那敏 4种组分制成的抗感冒复方制剂。其质量标准收载于山东、上海、四川等地方标准[1～ 3] 。现质量标准仅控制对乙酰氨基酚和咖啡因的含量。为完善其质量标准 ,控制产品质量 ,本文采用离子对色谱法同时测定感冒灵胶囊中 4种组分的含量 ,方法简便 ,准确。1　仪器与试药美国ＴＳＰ公司液相色谱系统 :包括Ｐ2 0 0 0二元梯度泵 ,ＡＳ30 0 0自动进样系统 ,ＵＶ2 0 0 0紫外检测器 ,工作站 (ＯＳ/ 2平台 /ＰＣ10 0 0数据处理软件 )。Ｆｉｎｎｐｉｐｅｔｔｅ芬兰数字显示移…     

Enhancement of tumor formation in mouse lung by dietary butylated hydroxytoluene

Male A/J mice were injected i.p. with a single dose of urethan and fed 0.75% butylated hydroxytoluene (BHT), butylated hydroxyanisole (BHA) or ethoxyquin in the diet. All animals were killed 4 months after urethan and the number of lung tumors counted. Exposure to BHT, but not to BHA or ethoxyquin significantly enhanced formation of lung tumors if animals were given the BHT-containing diet once a week for 8 consecutive weeks or were kept on it continuously for 8 weeks. Prefeeding mice with BHT had no effect on tumor formation but prefeeding BHA reduced the number of tumors formed by urethan. It is concluded from this and previous work that in mouse lung BHT enhances tumor formation regardless of route of administration and over a 100-fold dose range.     

Effects of butylated hydroxyanisole and butylated hydroxytoluene on dna adduct formation and arylamine N‐acetyltransferase activity in human bladder tumour cells

In this study, butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) were used to determine the inhibition of arylamine N‐acetyltransferase (NAT) activity and DNA adduct formation in human bladder tumour cell line T‐24. The activity of NAT was measured by high‐performance liquid chromatography, assaying for the amounts of N‐acetyl‐2‐aminofluorene and N‐acetyl‐p‐aminobenzoic acid and remaining 2‐aminofluorene and p‐aminobenzoic acid. Human bladder tumour cell line T‐24 cytosols and intact cells were used for examining NAT activity and carcinogen–DNA adduct formation. The results demonstrated that NAT activity and 2‐aminofluorene–DNA adduct formation in human bladder tumour cells were inhibited and decreased by BHA and BHT in a dose‐dependent manner. The effects of BHA and BHT on the values of the apparent K_m and V_max also were determined in both systems examined. The results indicated that BHA and BHT decreased the apparent values of K_m and V_max from human bladder tumour cells in both cytosol and intact cells. Copyright © 2002 John Wiley & Sons, Ltd.     

Cytotoxicity of butylated hydroxyanisole and butylated hydroxytoluene in isolated rat hepatocytes

The effects of the antioxidants butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) on isolated rat hepatocytes were investigated. Both antioxidants were observed to be cytotoxic in a concentration-dependent manner at concentrations ranging from 100 to 750 microM. At equimolar concentrations BHT was more cytotoxic than BHA. Their toxicity appeared to be independent of their metabolism to reactive intermediates since inhibitors of cytochrome P-450 (metyrapone, SKF 525-A and piperonyl butoxide) had no effect on the cytotoxicity and N-acetylcysteine was also without protective effect. In addition, deuterated BHT was equitoxic with BHT. Only low temperature incubation (4 degrees), which has previously been shown to inhibit the insertion of these compounds into biomembranes, was effective in inhibiting the cytotoxic effects. Using isolated rat liver mitochondria we observed that both BHA and BHT inhibited respiratory control primarily by stimulating state 4 respiration and thus acting as membrane uncouplers. BHA and BHT also effectively dissipated membrane potential across the mitochondrial membrane and caused the release of calcium and mitochondrial swelling. These mitochondrial effects were reflected by a rapid decrease in ATP levels in intact hepatocytes which preceded cell death. These results suggest that the observed cytotoxicity of BHA and BHT to hepatocytes is related to their effects on biomembranes and mitochondrial bioenergetics.     

药用丁基胶塞中抗氧剂BHT的UPLC法测定

摘 要 目的：建立超高效液相色谱法（UPLC）测定药用丁基胶塞中的2,6 二叔丁基对甲基苯酚（BHT）的含量。方法: 采用二氯甲烷 甲醇（1 ∶〖KG-*4〗1）为提取溶剂,利用超高效液相色谱法对BHT含量进行测定。色谱柱：资生堂CAPCELLPAK C18 （200 mm×50 mm ,2 μm）;流动相：乙腈 水 异丙醇（55 ∶〖KG-*4〗35 ∶〖KG-*4〗10）;流速：0.4 ml ·min-1;检测波长：280 nm;柱温：40℃;进样量：3 μl。结果: 抗氧剂BHT在0.2 50.0 μg ·ml-1浓度范围内线性关系良好（r=0.999 9）,平均回收率97.3%（RSD=1.4%,n=9）。结论: 该方法灵敏快速、结果准确,可用于测定药用丁基胶塞中BHT的含量。     

A new metabolite of butylated hydroxyanisole in man

Butylated hydroxyanisole (I) is one of the most commonly used food antioxidants. Its use has been suggested to inhibit a variety of carcinogenic responses. The present study on the disposition kinetics of (I) in man indicates that contrary to previous reports, (I) undergoes significant O-demethylation in the body yielding a tert-butyl hydroquinone. It is suggested that this metabolic conversion may be responsible for some of the in vivo activities of (I) against chemical carcinogens.     

超高效液相色谱法测定唐解胶囊中非法添加降糖类化学药物

目的 超高效液相色谱法测定唐解胶囊中降糖类化学药物含量.方法 采用Agillent Zorbax SB-C18(2.1 mm×50 mm,1.8 μm),二极管阵列检测器,检测波长为235 nm,流速为0.3 mL·min-1,流动相A为0.1%甲酸水溶液,流动相B为乙腈,按梯度进行洗脱.结果 盐酸苯乙双胍、罗格列酮和格列本脲分别在6.1~122、5.15~103、5.35~107 μg·mL-1范围内呈现良好的线性关系,平均精密度RSD(n=6)分别为0.86%、1.03%、0.52%,平均回收率分别为97.1%、97.5%、97.0%,RSD(n=6)分别为0.46%、1.04%、0.66%.结论 该方法前处理简单、分析时间短、灵敏度高、重现性好,可用于降糖类化学药物非法添加检测.     

Safety assessment of butylated hydroxyanisole and butylated hydroxytoluene as antioxidant food additives.

Butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) are widely used antioxidant food additives. They have been extensively studied for potential toxicities. This review details experimental studies of genotoxicity and carcinogenicity which bear on cancer hazard assessment of exposure to humans. We conclude that BHA and BHT pose no cancer hazard and, to the contrary, may be anticarcinogenic at current levels of food additive use.     

Toxicity studies of butylated hydroxyanisole and butylated hydroxytoluene. II. Chronic feeding studies

The antioxidants butylated hydroxyanisole (BHA) and butylated hydroxytoluene (BHT) were fed in the diet to male F344 rats in two chronic feeding studies. In one study, feeding BHT for 76 wk at concentrations ranging from 100 to 6000 ppm produced no increase in neoplasms at any site. In a second study, feeding 12,000 ppm BHT for 110 wk had no neoplastic effect at any site, whereas feeding BHA at 12,000 ppm resulted in a small increase in squamous cell papillomas of the non-glandular squamous portion of the stomach.     

The acute toxicity of butylated hydroxytoluene and its metabolites in mice

The acute toxicity of butylated hydroxytoluene (BHT) and four of its metabolites, 2,6-di-tert-butyl-4-hydroperoxy-4-methyl-2,5-cyclohexadien- 1-one(BHT-OOH), 2,6-di-tert-butyl-4-hydroxy-4-methyl-2,5-cyclohexadien- 1-one(BHT-OH), 2,6-di-tert-butyl-p-benzoquinone (DBQ), and 2,6-di-tert- butyl-4-[(methylthio)methyl] phenol (BHT-SCH₃) was studied in young male mice following intraperitoneal administration. The i.p. LD₅₀ values of BHT, BHT-OOH, BHT-OH, DBQ, and BHT-SCH₃ were 3550,190, above 1600, 2270, and 1840 $\text{mg}\text{kg}$, respectively. These results suggest that BHT-OOH probably is the most toxic metabolite of BHT.     

Estimate of the maximal daily dietary intake of butylated hydroxyanisole and butylated hydroxytoluene in The Netherlands

The daily dietary intake of the phenolic antioxidants butylated hydroxyanisole (BHA) and/or butylated hydroxytoluene (BHT) was estimated using data obtained from a nationwide dietary record survey carried out in The Netherlands in 1987/1988. The estimates were based on the fat content of selected food categories and their respective maximum permitted levels of BHA and/or BHT. The results indicate that it is unlikely that the current acceptable daily intake for BHA (0-0.05 mg/kg body weight) is surpassed, even in individuals with an extremely high caloric intake, except in extreme cases in 1-6-year-olds. However, it cannot be excluded that the acceptable daily intake for BHT (FAO/WHO: 0-0.125 mg/kg; EEC: 0-0.05 mg/kg) is exceeded in all age and sex groups, but particularly in children aged 1-6 years.