View More View Less
  • 1 College of Chemistry and Chemical Engineering, Yantai University, Yantai, , PR China
Open access

Abstract

A sweeping micellar electrokinetic chromatography (sweeping-MEKC) method was developed for the determination of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol in cosmetics. Several parameters affecting sweeping-MEKC method were studied systematically and the separation conditions were optimized as 20 mM NaH2PO4–110 mM SDS and 40% (v/v) MeOH (pH 2.4), with −22 kV applied voltage and UV detection at 230 nm. The sample matrix is 60 mmol L−1 NaH2PO4 and sample introduction was performed at 3 psi for 6 s. Separation of the four naphthalenediols was completed in less than 17 min. Limit of detection (LOD) and limit of quantitation (LOQ) are 0.0045∼0.0094 μg mL−1 and 0.015∼0.031 μg mL−1. Linear relationship (r 2 > 0.999) is satisfactory at the range of 0.1–10 μg mL−1. The developed method has been successfully applied to the determination of the four naphthalenediols in real cosmetic samples, with recoveries in foundation, sun cream and lotion in the range of 92.3%∼106.8% and relative standard deviation (RSD) less than 4.15%. A HPLC method described in the National Standards of the People’s Republic of China was carried out for the comparison with the proposed method. The results showed that the proposed sweeping-MEKC method has the advantages of fast, low cost with comparative sensitivity.

Abstract

A sweeping micellar electrokinetic chromatography (sweeping-MEKC) method was developed for the determination of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol in cosmetics. Several parameters affecting sweeping-MEKC method were studied systematically and the separation conditions were optimized as 20 mM NaH2PO4–110 mM SDS and 40% (v/v) MeOH (pH 2.4), with −22 kV applied voltage and UV detection at 230 nm. The sample matrix is 60 mmol L−1 NaH2PO4 and sample introduction was performed at 3 psi for 6 s. Separation of the four naphthalenediols was completed in less than 17 min. Limit of detection (LOD) and limit of quantitation (LOQ) are 0.0045∼0.0094 μg mL−1 and 0.015∼0.031 μg mL−1. Linear relationship (r 2 > 0.999) is satisfactory at the range of 0.1–10 μg mL−1. The developed method has been successfully applied to the determination of the four naphthalenediols in real cosmetic samples, with recoveries in foundation, sun cream and lotion in the range of 92.3%∼106.8% and relative standard deviation (RSD) less than 4.15%. A HPLC method described in the National Standards of the People’s Republic of China was carried out for the comparison with the proposed method. The results showed that the proposed sweeping-MEKC method has the advantages of fast, low cost with comparative sensitivity.

Introduction

In organic synthesis, 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol are important pharmaceutical intermediates, and the dosage must be strictly controlled [1–3]. 2,7-Naphthalenediol is a raw material for the synthesis of sulfonic acid compounds and divinyl naphthalene compounds in chemical production, while 1,5-naphthalenediol plays an important role in biochemical research [4, 5]. 1,7-Naphthalenediol and 2, 3-naphthalenediol are prohibited components in cosmetics, while the addition of 2,7-naphthalenediol and 1,5-naphthalenediol is strictly controlled [6]. Long-term excessive exposure to naphthalenediols can cause serious irritation to respiratory system and eyes, and may cause skin allergies [7, 8]. Therefore, it is necessary to establish a simple and efficient separation method to determine the content of the four naphthalenediols. The structures of the four naphthalenediols are given in Fig. 1.

Fig. 1.
Fig. 1.

The chemical structures of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol

Citation: Acta Chromatographica 2021; 10.1556/1326.2021.00942

High performance liquid chromatography (HPLC) is an existing method for the determination of naphthalenediols, which is considered to be a simple and feasible method for the determination of naphthalenediols [9–13]. Capillary electrophoresis (CE) is known as an environmental friendly method with high efficiency, short separation time and low reagent consumption [14, 15]. However, the small injection volume causes poor concentration sensitivity, which limits the usefulness of CE for trace analysis. Therefore, it is an urgent problem for electrophoresis workers to improve the sensitivity of CE. The on-line enrichment technology is a method of concentrating samples in the process of separation. The most common on-line enrichment methods are field amplification [16–18], sweeping [19–21] and isokinetic electrophoresis stacking [22–24]. Sweeping, a technique used in micellar electrokinetic chromatography (MEKC), is the picking and accumulation of the analytes by the pseudo stationary phase (PSP) that penetrates the sample zone containing no PSP during application of voltage. Sweeping-MEKC has been successfully applied to many analytical fields. However, the method of determination of the four naphthalenediols in cosmetics by sweeping-MEKC has not been reported.

In this work, a sweeping-MEKC method was established for on-line enrichment and separation of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol in cosmetics. A comparison with a HPLC method described in the national standard of the People’s Republic of China [25] was also carried out. The results showed that the established sweeping-MEKC method has the advantages of fast, low cost with comparative sensitivity.

Experimental

Chemicals and materials

1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol were purchased from Beijing Manhage Bio-Technology Company (Beijing, China). Foundation, sun cream and lotion were obtained from the supermarket nearby. Methanol and phosphoric acid were of chromatographic grade and were purchased from Kemel Chemical Reagent Co., Ltd (Tianjin, China). Acetic acid and 95% ethanol were purchased from Northern Tianyi Chemical Reagent Factory (Tianjin, China) and Yongda Chemical Reagent Co., Ltd. (Tianjin, China). Disodium hydrogen phosphate (NaH2PO4.2H2O, ≥99.0%) and sodium hydroxide (NaOH) were of analytical grade and were obtained from Sinopharm Chemical Reagent Co., Ltd (Shanghai, China). Sodium dodecyl sulfate (SDS) was purchased from Shanghai Macklin Biochemical Co., Ltd (Shanghai, China).

The standard stock solutions were prepared by dissolving the four naphthalenediols in MeOH respectively with the concentration of 100 μg ml−1. They were stored in a refrigerator at 4 °C. 0.5 g (accurate to 0.001 g) foundation, sun cream and lotion samples were added in a 10 ml plug colorimetric tube respectively. 4 ml MeOH were added to the samples and mixed well on a vortex oscillator. Then kept in an ultrasonic bath for 15 min. After the temperature of solution reached room temperature MeOH were added to fix the volume to 5 ml. 2 ml sample solution were taken in a centrifuge tube and centrifuged at 6,996×g for 2 min. After centrifugation, 1 ml sample was blown dry with nitrogen and reconstituted with 1 ml 60 mM NaH2PO4. Finally, the samples were filtered through microporous nylon filters with a pore size of 0.22 μm prior to use.

Apparatus

The SCIEX P/ACE™ MDQ plus CE system (Fullerton, CA) equipped with a diode array detector (DAD) and a fused silica capillary (Yongnian Photoconductive Fiber Factory, Hebei, China), with an i.d. of 75 μm and an o.d. of 375 μm were used. The total length of the capillary was 50.2 cm and the effective length was 40 cm. The HPLC system consisted of a Waters e2695 pump, a Waters 2998 PDA detector and an Empower chromatography management system (Waters, Milford Massachusetts, USA). A C18 reverse phase column (Tianyuan Technology Co., Ltd., Tianjin, China; Aces aqC18, 5 μm, 250 x 4.6 mm) was used. Data acquisition was performed using Karat 32 software (Beckman-Coulter, Fullerton, CA, USA).

Sweeping-MEKC conditions

Before the first use, new capillaries were conditioned with 1 mol L−1 NaOH for 20 min, Milli-Q water for 15 min and buffer for 30 min. At the beginning of every day, the capillary was washed with 1 mol L−1 NaOH, water and running buffer for 5 min, 5 min and 10 min, respectively. The detection wavelength of was set at 230 nm, and the temperature of the capillary was maintained at 25 °C. All solutions were filtered through microporous nylon filters with a pore size of 0.22 μm prior to use. Between runs, the capillary was rinsed with running buffer for 5 min. Samples were injected at a pressure of 3 psi (1 psi = 6,894.76 Pa) for 6 s. Working stock solutions were diluted with a sample matrix of 60 mM NaH2PO4 without SDS. The running buffer was composed of 20 mM NaH2PO4, 110 mM SDS and 40% (v/v) MeOH (pH 2.4). In this work, acidic buffer solution with low pH was used, so that the electroosmotic flow (EOF) could be ignored. During the separation, a reverse voltage of −22 kV was applied (negative injection). As the PSP, SDS micelles with negative charge move toward the positive electrode (detection window), whose electrophoretic speed is faster than that of the uncharged naphthalenediols. During the application of voltage, the PSP in background electrolyte solution (BGE) penetrates the sample region and the sample band of the analyte narrows.

To estimate the sensitivity increase achieved by using the sweeping-MEKC method, sensitivity enhancement factors (EF) based on peak area were estimated from the following equation:
EF=AsweptAMEKC
where A swept and A MEKC are the peak areas of the analytes after sweeping-MEKC and conventional MEKC in which separation conditions were optimized as 20 mM Na2B4O7, 50 mM SDS, pH 9.8, with 22 kV applied voltage, UV detection at 230 nm, and samples were injected at a pressure of 0.5 psi for 5 s.

HPLC conditions

The mobile phase was composed of methanol and 0.1% acetic acid solution for gradient elution with a 25–55% linear gradient of methanol from 0 to 35 min at a flow rate of 1.0 mL min−1 according to the National Standards of the People’s Republic of China (GB/T 35829-2018) [25]. All analyses were performed at room temperature with the PDA detection wavelength of 230 nm. The samples were prepared in the same manner as for MEKC analysis except for reconstitution with 60 mM NaH2PO4. MeOH solvent was used for samples instead of matrix solution. The volume of every sample injected into the column was 10 µL.

Results and discussion

Optimization of sweeping-MEKC separation conditions

Optimization of sample injection time. For sweeping-MEKC, the injected length of the sample zone is restricted by the value of 1/(1+k), where k is the capacity factor of the analyte. Only the column length restricts the length of injection when k goes to infinity. The sample length of injection is suggested to be optimized when the k value of the analyte is not high [26]. In this work, 110 mmol L−1 SDS, 20 mmol L−1 NaH2PO4 (pH 2.4) containing 35% MeOH were used as buffer solution and the sample matrix was 60 mmol L−1 NaH2PO4. The sample solution was injected at 3 psi for 6, 8 and 10 s into the column. From Fig. 2, we can see that the peak areas of the analytes increased with the increase of sample injection time. However, the peak of the four naphthalenediols split when the sample injection time increased to 8 and 10 s. The reason is that the sweeping performance is influenced by injected sample volume, and with the increasing of sample injection time, the PSP is not sufficient enough to sweep all the analytes and the peaks split. At 6 s, the peak shape and the resolution of the four naphthalenediols is relatively satisfactory. Therefore, we chose 6 s as the best injection time at 3 psi.

Fig. 2.
Fig. 2.

Effect of injection time on the sweeping efficiency for the four naphthalenediols. Sweeping-MEKC conditions: 20 mM NaH2PO4–110 mM SDS containing 35%MeOH, pH 2.4, pressure injection with 3 psi, −20 kV applied voltage, UV detection at 230 nm. Sample matrix: 60 mM NaH2PO4. Peak: (1) 2,3-naphthalenediol (2) 1,7-naphthalenedio (3) 2,7-naphthalenediol (4) 1,5-naphthalenediol

Citation: Acta Chromatographica 2021; 10.1556/1326.2021.00942

Optimization of organic modifier. The addition of organic modifier can impact the distribution of the analytes between micelles and buffer solution, which can improve the separation degree and peak shape of the analytes. It can also increase the solubility of the analytes. In this work MeOH was used as organic modifier and the effect of the content of MeOH in the range of 30%–45% on the separation and enrichment of the four naphthalenediols was investigated. As shown in Fig. 3, baseline separations were obtained under the four MeOH levels. However, the last peak (1,5-naphthalenediol) has obvious shoulder in front when the content of MeOH were 30% and 35%. In addition, with the increase of MeOH content, the migration times of the four naphthalenediols prolonged. Given full consideration of the peak shape and separation time, 40% MeOH was chosen.

Fig. 3.
Fig. 3.

Effect of organic modifier on the separation of the four naphthalenediols. Sweeping-MEKC conditions: 20 mM NaH2PO4–110 mM SDS, pH 2.4, pressure injection 6 s with 3 psi, −20 kV applied voltage, UV detection at 230 nm. Sample matrix: 60 mM NaH2PO4. Peak identification: as in Figure 2.

Citation: Acta Chromatographica 2021; 10.1556/1326.2021.00942

Optimization of the concentration of SDS. The analyte with higher retention factor has better sweeping efficiency, while one of the factors affecting the retention factor is the concentration of PSP in BGE. To investigate the influence of SDS concentration on separation, experiments were carried out using 20 mM NaH2PO4 containing 40% MeOH at pH 2.4 with different concentrations of SDS (80∼120 mM). As shown in Fig. 4, with the increase of SDS concentration, the migration time of analytes decreased slightly because more and more of the analytes were incorporated into the micellar phase. Considering the migration time, peak shape and peak area, 110 mM SDS was used.

Fig. 4.
Fig. 4.

Effect of SDS concentration on the separation of the four naphthalenediols. Sweeping-MEKC conditions: 20 mM NaH2PO4 containing 40%MeOH, pH 2.4, pressure injection 6 s with 3 psi, −20 kV applied voltage, UV detection at 230 nm. Sample matrix: 60 mM NaH2PO4. Peak identification: as in Figure 2.

Citation: Acta Chromatographica 2021; 10.1556/1326.2021.00942

Optimization of the running buffer concentration and sample matrix composition. Generally, phosphate solutions are used as buffer solutions with low pH. The effect of the concentration of running buffer on the separation of the four naphthalenediols in the range of 10∼40 mM is illustrated in Fig. 5 (A). We can see that changing the concentration of NaH2PO4 has little effect on the migration time of the four naphthalenediols. The sensitivity and peak area of the analytes are the highest at 20 mM NaH2PO4. Therefore, 20 mM NaH2PO4 was chosen. Since the sample matrix could affect the degree of sample stacking, we need to investigate the concentration of it. The sample matrix is composed of NaH2PO4 solution without SDS and the effect of the concentrations from 40 to 100 mM on sweeping was investigated. The results in Fig. 5 (B) indicated that the highest peak intensity of naphthalenediols was achieved using 60 mM NaH2PO4 as the sample matrix solution.

Fig. 5.
Fig. 5.

Effect of (A) buffer concentration (B) and sample matrix composition on the sweeping efficiency for the four naphthalenediols. Sweeping-MEKC conditions: the concentration of NaH2PO4 indicated in Figure 5(A) with 110 mM SDS and 40%MeOH (pH=2.4); other conditions as in Figure 4. Peak identification: as in Figure 2.

Citation: Acta Chromatographica 2021; 10.1556/1326.2021.00942

Optimization of separation voltage. Separation voltage is also a very important parameter in sweeping-MEKC. Usually higher voltage is needed to make sweeping-MEKC fast and efficient. The effect of different voltages (−20, −22, −24 and −26 kV) on the separation of the analytes was investigated by using a running buffer consisting of 20 mM NaH2PO4–110 mM SDS and 40%MeOH at pH 2.4. As shown in Fig. 6, with the increase of voltage the migration time of the analytes became shorter gradually. When the applied voltage was higher than −22 kV the last peak (1,5-naphthalenediol) had obvious shoulder in front. So −22 kV was used.

Fig. 6.
Fig. 6.

Effect of separation voltage on the analysis of the four naphthalenediols. Sweeping-MEKC conditions: 20 mM NaH2PO4–110mM SDS containing 40%MeOH, pH 2.4, pressure injection 6 s with 3 psi, UV detection at 230 nm. Sample matrix: 60 mM NaH2PO4. Peak identification: as in Figure 2.

Citation: Acta Chromatographica 2021; 10.1556/1326.2021.00942

To sum up, the optimum conditions are as follows: BGE composed of 20 mM NaH2PO4–110 mM SDS, and 40% (v/v) MeOH (pH 2.4); sample matrix composed of 60 mM NaH2PO4; sample was injected by pressure injection at 3 psi for 6 s. The corresponding electropherogram of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol mixed standard solution obtained under the optimized conditions is shown in Fig. 7 (A). The retention time of 2,3-naphthalenediol, 1,7-naphthalenediol, 2,7-naphthalenediol and 1,5-naphthalenediol is 12.10 min, 13.56 min, 15.27 min and 16.68 min, respectively.

Fig. 7.
Fig. 7.

Typical (A) electropherogram and (B) chromatogram of 5 μg/mL for the four naphthalenediols. Peak: (1) 2,3-naphthalenediol (2) 1,7-naphthalenedio (3) 2,7-naphthalenediol (4) 1,5-naphthalenediol. Sweeping-MEKC conditions: 20 mM NaH2PO4·2H2O –110 mM SDS containing 40% MeOH at pH 2.4, pressure injection 6 s with 3 psi, −22 kV applied voltage, UV detection at 230 nm. HPLC conditions: mobile phase, methanol and 0.1% acetic acid solution were eluted in a gradient, 1.0 mL·min–1 flow rate, UV detection at 230nm.

Citation: Acta Chromatographica 2021; 10.1556/1326.2021.00942

HPLC method

The four naphthalenediols were analyzed by the HPLC method as described in the National Standard of the People’s Republic of China (GB/T 35829-2018) and the result is shown in Fig. 7 (B). The retention time of 1,5-naphthalenediol, 2,7-naphthalenediol, 1,7-naphthalenediol and 2,3-naphthalenediol is 16.33 min, 20.30 min, 25.64 min and 28.09 min respectively. From Fig. 7, we can see that the separation time of the four analytes by using the HPLC method is longer than that with the sweeping-MEKC method.

Validation of Sweeping-MEKC and HPLC methods

To verify both the sweeping-MEKC and HPLC methods, system suitability, linearity, LOD, LOQ, EF and precision were extensively validated.

System suitability. The values of migration/retention time (t), tailing factor (T) and theoretical plates (N) were evaluated by using six replicate injections of a same mixed standard solution of the analytes. The results obtained are listed in Table 1.

Table 1.

Results of system suitability tests for analysis of the four naphthalenediols (n = 6)ab

MethodAnalytesMigration/retention

time, (min)
Tailing factorTheoretical plate number
sweeping-MEKC1,7-naphthalenediol13.56 ± 0.160.94 ± 0.0370809
2,3-naphthalenediol12.10 ± 0.150.94 ± 0.0297129
1,5-naphthalenediol16.68 ± 0.160.93 ± 0.0238534
2,7-naphthalenediol15.27 ± 0.140.91 ± 0.0454716
HPLC1,7-naphthalenediol26.64 ± 0.161.06 ± 0.0332382
2,3-naphthalenediol28.09 ± 0.140.90 ± 0.027706
1,5-naphthalenediol16.33 ± 0.121.06 ± 0.0212261
2,7-naphthalenediol20.30 ± 0.0841.07 ± 0.0416612

a Values are means of six measurements ± SD.

b Concentration of 5 μg mL−1 individual for the four naphthalenediols was chosen for the assays of system suitability.

Linearity, LOD, LOQ and EF. The results obtained are summarized in Table 2. The EFs of 2,3-naphthalenediol, 1,7-naphthalenediol, 2,7-naphthalenediol and 1,5-naphthalenediol are 32, 29, 56 and 42, respectively. From Table 2 we can conclude that there is good (r 2 > 0.999) linear correlations between the concentration of the four naphthalenediols and the corresponding peak areas by both sweeping-MEKC and HPLC methods. The limit of detection (LOD) and the limit of quantitation (LOQ) were obtained as three and ten times of the signal-to-noise ratio (S/N) respectively. The LODs obtained by sweeping-MEKC method were 0.0045∼0.0094 μg mL−1 and 0.0085∼0.018 μg mL−1 by HPLC method. The LOQs obtained were 0.015∼0.031 μg mL−1 by sweeping-MEKC method and 0.028∼0.060 μg mL−1 by HPLC method.

Table 2.

Linear, LOD and LOQ data for the analysis of the four naphthalenediols by sweeping-MEKC and HPLC

MethodAnalytesCalibration curveaCorrelation

Coefficient (r2)
Linear range (µg·mL−1)LOD (µg·mL−1)LOQ (µg·mL−1)EF
sweeping-MEKC1,7-naphthalenedioly = 39363x+1027.50.9990.1–100.00750.02529
2,3-naphthalenedioly = 62514x−3583.20.9990.1–100.00450.01532
1,5-naphthalenedioly = 65990x−2027.50.9990.1–100.00940.03142
2,7-naphthalenedioly = 65578x−304.960.9990.1–100.00690.02356
HPLC1,7-naphthalenedioly = 130285x+129040.9990.75–200.0180.060-
2,3-naphthalenedioly = 264155x+75530.9990.75–200.00980.033-
1,5-naphthalenedioly = 166698x+111550.9990.75–200.0120.040-
2,7-naphthalenedioly = 206908x+403280.9990.75–200.00850.028-

a y and x stand for the peak area and the concentration (µg·mL−1) of the four naphthalenediols, respectively.

Intra-day precision and inter-day precision. The intra-day precision and inter-day precision were obtained by injecting the same mixed standard solution for 6 times on one day and 6 consecutive days respectively. The relative standard deviations (RSDs) were calculated for both the migration/retention time and the peak area of the four analytes for evaluation, and the results were satisfactory. The results are listed in Table 3.

Table 3.

Precision for analysis of the four naphthalenediols by sweeping-MEKC and HPLC (n = 6)a

RSD (%)
MethodAnalytesIntra-dayInter-day
Migration/retention timePeak areaMigration/retention timePeak area
sweeping-MEKC1,7-naphthalenediol1.180.822.133.05
2,3-naphthalenediol1.241.061.762.84
1,5-naphthalenediol1.081.251.972.65
2,7-naphthalenediol0.921.082.383.73
HPLC1,7-naphthalenediol0.600.921.322.31
2,3-naphthalenediol0.490.851.542.24
1,5-naphthalenediol0.730.721.652.56
2,7-aphthalenediol0.410.871.272.18

a Concentration of 5 μg mL−1 individual for the four naphthalenediols was chosen for the assays of system suitability.

Sample analysis

Under the optimized conditions, three different kinds of cosmetic samples i.e. foundation, sun cream and lotion (marked as A, B and C) were analyzed by both sweeping-MEKC and HPLC methods. Typical electropherograms and chromatograms of all the cosmetic samples are shown in Fig. 8. From Fig. 8 we can see that no naphthalenediols in the blank samples of the three cosmetics were detected by both two methods. As mentioned in the introduction, 1,7-naphthalenediol and 2,3-naphthalenediol are prohibited components in cosmetics and the addition of 1,5-naphthalenediol and 2,7-naphthalenediol are strictly limited. That’s why there is no signal response of the four naphthalenediols. To further evaluate the performance of the proposed method in complex matrices and verify the accuracy of both two methods, standards of the four naphthalenediols at concentrations of 0.5 μg mL−1 and 1.0 μg mL−1 were added to the real cosmetic samples. The recoveries of them obtained were 92.3%∼106.8% by sweeping-MEKC method and 90.4%∼107.5% by HPLC method. The results are listed in Table 4.

Fig. 8.
Fig. 8.

Electropherograms (A1, B1, C1) of three samples: none-spiked (a), spiked with 0.5 μg·mL–1 (b), spiked with 1.0 μg·mL–1 (c); and chromatograms (A2, B2, C2) of three samples: none-spiked (a), spiked with 0.5 μg·mL–1 (b), spiked with 1.0 μg·mL–1 (c); Peak: (1) 2,3-naphthalenediol (2) 1,7-naphthalenediol (3) 2,7-naphthalenediol (4) 1,5-naphthalenediol (A1, A2) foundation, (B1, B2) sun cream, (C1, C2) lotion, other conditions are same as those in Figure 7.

Citation: Acta Chromatographica 2021; 10.1556/1326.2021.00942

Table 4.

The recoveries of the four naphthalenediols in three samples by sweeping-MEKC and HPLC methods (n = 3)

MethodSampleAnalytesOriginal amount (µg·mL−1)Added (µg·mL−1)Found ± SD (µg·mL−1)Recovery (%)RSD (%)
sweeping-MEKCFoundation1,7-naphthalenediola0.50.49 ± 0.01697.73.21
1.00.98 ± 0.02598.22.56
2,3-naphthalenediol0.50.48 ± 0.008951.67
1.01.02 ± 0.023101.32.31
1,5-naphthalenediol0.50.52 ± 0.011104.22.12
1.00.94 ± 0.03494.13.58
2,7-naphthalenediol0.50.46 ± 0.01992.34.15
1.01.05 ± 0.041105.03.98
Sun cream1,7-naphthalenediol0.50.53 ± 0.015106.82.87
1.00.97 ± 0.03796.73.84
2,3-naphthalenediol0.50.48 ± 0.00996.81.83
1.00.93 ± 0.02193.22.25
1,5-naphthalenediol0.50.48 ± 0.02098.74.02
1.00.98 ± 0.02997.52.92
2,7-naphthalenediol0.50.52 ± 0.016102.53.01
1.00.95 ± 0.01895.31.87
Lotion1,7-naphthalenediol0.50.49 ± 0.01398.32.73
1.00.95 ± 0.02594.62.62
2,3-naphthalenediol0.50.52 ± 0.011102.32.04
1.01.06 ± 0.021106.01.97
1,5-naphthalenediol0.50.48 ± 0.01796.43.57
1.00.98 ± 0.04098.54.13
2,7-naphthalenediol0.50.53 ± 0.020105.63.78
1.00.92 ± 0.02092.32.19
HPLCFoundation1,7-naphthalenediol0.50.47 ± 0.004294.00.89
1.01.04 ± 0.0094104.30.90
2,3-naphthalenediol0.50.53 ± 0.0096106.21.81
1.01.05 ± 0.012105.41.14
1,5-naphthalenediol0.50.45 ± 0.004790.41.04
1.00.93 ± 0.007492.80.80
2,7-naphthalenediol0.50.48 ± 0.004296.00.88
1.00.96 ± 0.01295.91.25
Sun cream1,7-naphthalenediol0.50.52 ± 0.0022103.50.42
1.00.95 ± 0.008294.60.86
2,3-naphthalenediol0.50.52 ± 0.0045103.70.87
1.00.95 ± 0.01495.21.47
1,5-naphthalenediol0.50.53 ± 0.0062105.81.17
1.01.07 ± 0.0075106.70.70
2,7-naphthalenediol0.50.54 ± 0.0043107.50.80
1.00.94 ± 0.008294.40.87
Lotion1,7-naphthalenediol0.50.46 ± 0.007491.71.61
1.01.04 ± 0.012103.81.15
2,3-naphthalenediol0.50.47 ± 0.004494.20.94
1.00.96 ± 0.007295.80.75
1,5-naphthalenediol0.50.47 ± 0.005494.11.15
1.01.03 ± 0.0074102.60.72
2,7-naphthalenediol0.50.47 ± 0.005293.81.11
1.01.04 ± 0.0072104.40.69

a Not detected.

Comparison of MEKC and HPLC methods

Based on the results given above we can see that both methods can be successfully applied to the determination of the content of the four naphthalenediols in cosmetics. Combined with the on-line concentration sweeping strategy, the MEKC method can achieve even lower LODs and LOQs than those of the HPLC method. Furthermore, the developed sweeping-MEKC method has the advantages of lower reagent consumption, faster separation speed, and higher theoretical plate number, which can be potentially considered as an alternative to the existing HPLC methods in cosmetic naphthalenediol analysis.

Conclusion

In this work, an efficient sweeping-MEKC method for the analysis of 1,7-naphthalenediol, 2,3-naphthalenediol, 1,5-naphthalenediol and 2,7-naphthalenediol has been developed and verified. The four naphthalenols in cosmetics could be determined within shorter separation time with comparable sensitivity compared with the HPLC method. The present study shows that sweeping-MEKC is a powerful analytical tool for rapid screening of the four naphthalenediols in cosmetics.

Conflict of interest

The authors have no conflict of interest to declare.

Acknowledgments

We are grateful for the financial support from the National Natural Science Foundation of China (no. 51573155).

References

  • 1.

    Carvalho, L. M. ; Silva, A. M. S. ; Martins, C. I. ; Coelho, P. J. ; Oliveira-Campos, A. M. F. Tetrahedron Lett. 2003, 44, 19031905.

  • 2.

    Gupta, M. ; Mahajan, V. K. ; Mehta, K. S. ; Chauhan, P. S. Indian J. Dermatol. 2015, 6, 241246.

  • 3.

    Ren, H. ; Xiao, J. ; Chen, W. Polym. Plast. Technol. Eng. 2011, 50, 599603.

  • 4.

    Mezheritskii, V. V. ; Tyurin, R. V. ; Minyaeva, L. G. ; Antonov, A. N. ; Zadorozhnaya, A. P. Russ. J. Org. 2006, 42, 14581463.

  • 5.

    Nayak, U. K. S. Indian J. Dermatol. 2015, 6, 246247.

  • 6.

    Slitikov, P. V. ; Rasadkina, E. N. Russ. J. Org. 2016, 86, 544550.

  • 7.

    Stiborová, M. ; Frei, E. ; Schmeiser, H. H. ; Wiessler, M. ; Hradec, J. Cancer Lett. 1993, 68, 4347.

  • 8.

    Ge, Y. Y. ; Zhang, Q. ; Feng, H. J. ; Yao, S. ; Cheng, C. China Deterg. Cosmet. 2017, 40, 16.

  • 9.

    Huang, J. F. ; Lin, S. Y. ; He, M. H. ; Li, X. Y. ; Guo, X. D. ; Wu, Y. L. Mod. Food Sci. Tech. 2012, 28, 583587.

  • 10.

    Chen, L. ; Huang, J. ; He, M. ; Lin, S. ; Guo, X. Chin. J. Chromatogr. 2012, 30, 630634.

  • 11.

    Xu, L. Z. ; Li, X. Y. ; Xian, Y. P. ; He, M. H. ; Fang, J. ; Huang, J. F. ; Guo, X. D. J. Instrumental Anal. 2015, 34, 923927.

  • 12.

    Rao, Y. ; Guo, C. X. Chin. Pharm. 2007, 10, 158159.

  • 13.

    Yu, W. L. ; Zhao, K. L. ; Sun, X. ; Du, Z. X. Phys. Test. Chem. Anal. (Part B: Chem. Anal.). 2010, 46, 220223.

  • 14.

    Ma, J. ; Lu, W. ; Chen, L. Curr. Anal. Chem. 2012, 8, 7890.

  • 15.

    Wen, Y. ; Li, J. ; Ma, J. ; Chen, L. Electrophoresis 2012, 33, 29332952.

  • 16.

    Anres, P. ; Delaunay, N. ; Vial, J. ; Thormann, W. ; Gareil, P. Electrophoresis 2013, 34, 353362.

  • 17.

    Xin, H. ; Nauwelaers, T. ; Busson, R. ; Adams, E. ; Hoogmartens, J. ; Schepdael, A. V. Electrophoresis 2010, 31, 33523361.

  • 18.

    Zhao, Y. ; Mclaughlin, K. ; Lunte, C. E. Anal. Chem. 1998, 70, 45784585.

  • 19.

    Su, H. L. ; Feng, L. I. ; Jen, H. P. ; Hsieh, Y. Z. Electrophoresis 2008, 29, 42704276.

  • 20.

    Tsai, C. H. ; Chan, P. H. ; Lin, C. H. ; Chang, T. C. ; Chia, C. H. Electrophoresis 2006, 27, 46884693.

  • 21.

    Yang, Y. Y. ; Liu, J. T. ; Lin, C. H. Electrophoresis 2010, 30, 10841087.

  • 22.

    Procházková, A. ; Kivánková, L. ; Boček, P. J. Chromatogr. A. 1999, 838, 213221.

  • 23.

    Procházková, A. ; Krivánková, L. ; Boček, P. Electrophoresis 1998, 19, 300304.

  • 24.

    Shihabi, Z. K. Electrophoresis 2002, 23, 16121617.

  • 25.

    National Standards of the People’s Republic of China, GB/T 35829-2018.

  • 26.

    Quirino, J. P. ; Kim, J. B. ; Terabe, S. J. Chromatogr. A. 2002, 965, 357373.

  • 1.

    Carvalho, L. M. ; Silva, A. M. S. ; Martins, C. I. ; Coelho, P. J. ; Oliveira-Campos, A. M. F. Tetrahedron Lett. 2003, 44, 19031905.

  • 2.

    Gupta, M. ; Mahajan, V. K. ; Mehta, K. S. ; Chauhan, P. S. Indian J. Dermatol. 2015, 6, 241246.

  • 3.

    Ren, H. ; Xiao, J. ; Chen, W. Polym. Plast. Technol. Eng. 2011, 50, 599603.

  • 4.

    Mezheritskii, V. V. ; Tyurin, R. V. ; Minyaeva, L. G. ; Antonov, A. N. ; Zadorozhnaya, A. P. Russ. J. Org. 2006, 42, 14581463.

  • 5.

    Nayak, U. K. S. Indian J. Dermatol. 2015, 6, 246247.

  • 6.

    Slitikov, P. V. ; Rasadkina, E. N. Russ. J. Org. 2016, 86, 544550.

  • 7.

    Stiborová, M. ; Frei, E. ; Schmeiser, H. H. ; Wiessler, M. ; Hradec, J. Cancer Lett. 1993, 68, 4347.

  • 8.

    Ge, Y. Y. ; Zhang, Q. ; Feng, H. J. ; Yao, S. ; Cheng, C. China Deterg. Cosmet. 2017, 40, 16.

  • 9.

    Huang, J. F. ; Lin, S. Y. ; He, M. H. ; Li, X. Y. ; Guo, X. D. ; Wu, Y. L. Mod. Food Sci. Tech. 2012, 28, 583587.

  • 10.

    Chen, L. ; Huang, J. ; He, M. ; Lin, S. ; Guo, X. Chin. J. Chromatogr. 2012, 30, 630634.

  • 11.

    Xu, L. Z. ; Li, X. Y. ; Xian, Y. P. ; He, M. H. ; Fang, J. ; Huang, J. F. ; Guo, X. D. J. Instrumental Anal. 2015, 34, 923927.

  • 12.

    Rao, Y. ; Guo, C. X. Chin. Pharm. 2007, 10, 158159.

  • 13.

    Yu, W. L. ; Zhao, K. L. ; Sun, X. ; Du, Z. X. Phys. Test. Chem. Anal. (Part B: Chem. Anal.). 2010, 46, 220223.

  • 14.

    Ma, J. ; Lu, W. ; Chen, L. Curr. Anal. Chem. 2012, 8, 7890.

  • 15.

    Wen, Y. ; Li, J. ; Ma, J. ; Chen, L. Electrophoresis 2012, 33, 29332952.

  • 16.

    Anres, P. ; Delaunay, N. ; Vial, J. ; Thormann, W. ; Gareil, P. Electrophoresis 2013, 34, 353362.

  • 17.

    Xin, H. ; Nauwelaers, T. ; Busson, R. ; Adams, E. ; Hoogmartens, J. ; Schepdael, A. V. Electrophoresis 2010, 31, 33523361.

  • 18.

    Zhao, Y. ; Mclaughlin, K. ; Lunte, C. E. Anal. Chem. 1998, 70, 45784585.

  • 19.

    Su, H. L. ; Feng, L. I. ; Jen, H. P. ; Hsieh, Y. Z. Electrophoresis 2008, 29, 42704276.

  • 20.

    Tsai, C. H. ; Chan, P. H. ; Lin, C. H. ; Chang, T. C. ; Chia, C. H. Electrophoresis 2006, 27, 46884693.

  • 21.

    Yang, Y. Y. ; Liu, J. T. ; Lin, C. H. Electrophoresis 2010, 30, 10841087.

  • 22.

    Procházková, A. ; Kivánková, L. ; Boček, P. J. Chromatogr. A. 1999, 838, 213221.

  • 23.

    Procházková, A. ; Krivánková, L. ; Boček, P. Electrophoresis 1998, 19, 300304.

  • 24.

    Shihabi, Z. K. Electrophoresis 2002, 23, 16121617.

  • 25.

    National Standards of the People’s Republic of China, GB/T 35829-2018.

  • 26.

    Quirino, J. P. ; Kim, J. B. ; Terabe, S. J. Chromatogr. A. 2002, 965, 357373.

The author instruction is available in PDF.
Please, download the file from HERE.
 
The Open Access statement together with the description of the Copyright and License Policy are available in PDF.
Please, download the file from HERE.
 

 

Senior editors

Editor(s)-in-Chief: Kowalska, Teresa

Editor(s)-in-Chief: Sajewicz, Mieczyslaw

Editors(s)

  • Danica Agbaba (University of Belgrade, Belgrade, Serbia)
  • Ivana Stanimirova-Daszykowska (University of Silesia, Katowice, Poland)
  • Monika Waksmundzka-Hajnos (Medical University of Lublin, Lublin, Poland)

Editorial Board

  • R. Bhushan (The Indian Institute of Technology, Roorkee, India)
  • J. Bojarski (Jagiellonian University, Kraków, Poland)
  • B. Chankvetadze (State University of Tbilisi, Tbilisi, Georgia)
  • M. Daszykowski (University of Silesia, Katowice, Poland)
  • T.H. Dzido (Medical University of Lublin, Lublin, Poland)
  • A. Felinger (University of Pécs, Pécs, Hungary)
  • K. Glowniak (Medical University of Lublin, Lublin, Poland)
  • B. Glód (Siedlce University of Natural Sciences and Humanities, Siedlce, Poland)
  • U. Hubicka (Jagiellonian University, Kraków, Poland)
  • K. Kaczmarski (Rzeszow University of Technology, Rzeszów, Poland)
  • H. Kalász (Semmelweis University, Budapest, Hungary)
  • I. Klebovich (Semmelweis University, Budapest, Hungary)
  • A. Koch (Private Pharmacy, Hamburg, Germany)
  • Ł. Komsta (Medical University of Lublin, Lublin, Poland)
  • P. Kus (Univerity of Silesia, Katowice, Poland)
  • D. Mangelings (Free University of Brussels, Brussels, Belgium)
  • E. Mincsovics (Corvinus University of Budapest, Budapest, Hungary)
  • G. Morlock (Giessen University, Giessen, Germany)
  • A. Petruczynik (Medical University of Lublin, Lublin, Poland)
  • J. Sherma (Lafayette College, Easton, PA, USA)
  • R. Skibiński (Medical University of Lublin, Lublin, Poland)
  • B. Spangenberg (Offenburg University of Applied Sciences, Germany)
  • T. Tuzimski (Medical University of Lublin, Lublin, Poland)
  • Y. Vander Heyden (Free University of Brussels, Brussels, Belgium)
  • A. Voelkel (Poznań University of Technology, Poznań, Poland)
  • B. Walczak (University of Silesia, Katowice, Poland)
  • W. Wasiak (Adam Mickiewicz University, Poznań, Poland)

 

KOWALSKA, TERESA
E-mail: kowalska@us.edu.pl

SAJEWICZ, MIECZYSLAW
E-mail:msajewic@us.edu.pl

Indexing and Abstracting Services:

  • Science Citation Index
  • Sci Search
  • Research Alert
  • Chemistry Citation Index and Current Content/Physical
  • Chemical and Earth Sciences
  • SCOPUS
  • GoogleScholar
  • Index Copernicus
  • CABI
2020
 
Total Cites
650
WoS
Journal
Impact Factor
1,639
Rank by
Chemistry, Analytical 71/83 (Q4)
Impact Factor
 
Impact Factor
1,412
without
Journal Self Cites
5 Year
1,301
Impact Factor
Journal
0,34
Citation Indicator
 
Rank by Journal
Chemistry, Analytical 75/93 (Q4)
Citation Indicator
 
Citable
45
Items
Total
43
Articles
Total
2
Reviews
Scimago
28
H-index
Scimago
0,316
Journal Rank
Scimago
Chemistry (miscellaneous) Q3
Quartile Score
 
Scopus
393/181=2,2
Scite Score
 
Scopus
General Chemistry 215/398 (Q3)
Scite Score Rank
 
Scopus
0,560
SNIP
 
Days from
58
submission
 
to acceptance
 
Days from
68
acceptance
 
to publication
 
Acceptance
51%
Rate

2019  
Total Cites
WoS
495
Impact Factor 1,418
Impact Factor
without
Journal Self Cites
1,374
5 Year
Impact Factor
0,936
Immediacy
Index
0,460
Citable
Items
50
Total
Articles
50
Total
Reviews
0
Cited
Half-Life
6,2
Citing
Half-Life
8,3
Eigenfactor
Score
0,00048
Article Influence
Score
0,164
% Articles
in
Citable Items
100,00
Normalized
Eigenfactor
0,05895
Average
IF
Percentile
20,349
Scimago
H-index
26
Scimago
Journal Rank
0,255
Scopus
Scite Score
226/167=1,4
Scopus
Scite Score Rank
Chemistry (miscellaneous) 240/398 (Q3)
Scopus
SNIP
0,494
Acceptance
Rate
41%

 

Acta Chromatographica
Publication Model Online only
Gold Open Access
Submission Fee none
Article Processing Charge 400 EUR/article
Regional discounts on country of the funding agency World Bank Lower-middle-income economies: 50%
World Bank Low-income economies: 100%
Further Discounts Editorial Board / Advisory Board members: 50%
Corresponding authors, affiliated to an EISZ member institution subscribing to the journal package of Akadémiai Kiadó: 100%
Subscription Information Gold Open Access
Purchase per Title  

Acta Chromatographica
Language English
Size A4
Year of
Foundation
1992
Publication
Programme
2021 Volume 33
Volumes
per Year
1
Issues
per Year
4
Founder Institute of Chemistry, University of Silesia
Founder's
Address
PL-40-007 Katowice, Poland, Bankowa 12
Publisher Akadémiai Kiadó
Publisher's
Address
H-1117 Budapest, Hungary 1516 Budapest, PO Box 245.
Responsible
Publisher
Chief Executive Officer, Akadémiai Kiadó
ISSN 2083-5736 (Online)

Monthly Content Usage

Abstract Views Full Text Views PDF Downloads
Jun 2021 0 0 0
Jul 2021 0 0 0
Aug 2021 0 0 0
Sep 2021 0 113 27
Oct 2021 0 17 19
Nov 2021 0 62 15
Dec 2021 0 1 3