Nghiên cứu xác định đồng thời kẽm và gluconat trong thực phẩm bảo vệ sức khỏe bằng phương pháp CE-C4D

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Thông tin xuất bản: Tạp chí Kiểm nghiệm và An toàn thực phẩm, 2023

Mô tả vật lý: tr.280-294

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Các thực phẩm bảo vệ sức khỏe bổ sung vi chất cho cơ thể, như các nguyên tố kẽm (Zn), magnesi (Mg)… dưới các dạng muối dễ hấp thu như gluconat, sterat, lactat… ngày càng trở nên phổ biến. Tuy nhiên, một số loại tá dược (ví dụ các dạng muối vô cơ như kẽm sulfat, magnesi sulfat…) có chứa các nguyên tố này cũng thường được sử dụng trong quá trình bào chế. Vì vậy, nếu sử dụng các phương pháp phân tích tổng hàm lượng kim loại sẽ không đánh giá được chính xác hàm lượng các vi chất ở dạng muối dễ hấp thu, đặt ra yêu cầu phải phân tích đồng thời cả vi chất và các gốc muối để đánh giá đúng dạng muối bổ sung vào sản phẩm. Trong nghiên cứu này, phương pháp điện di mao quản với detector độ dẫn không tiếp xúc (CE-C4D) được sử dụng để xác định đồng thời hàm lượng Zn2+ và gluconat trong thực phẩm bảo vệ sức khỏe. Điều kiện phân tích được lựa chọn bao gồm: (1) đệm Tris/Ace 10 mM ở pH = 5,0
(2) mao quản silica đường kính trong 50 μm với chiều dài hiệu dụng 30 cm
(3) thế tách +15 kV
(4) bơm mẫu thủy động học kiểu xiphong ở chiều cao 10 cm trong 20 s. Phương pháp đạt được giới hạn phát hiện của Zn2+ và gluconat lần lượt là 1,0 mg/L và 1,5 mg/L. Phương pháp có độ chụm tốt (RSD <
3%) và độ đúng được đánh giá qua độ thu hồi tốt đối với Zn2+ (89-103%) và gluconat (88-107%). Phương pháp đã được áp dụng để xác định đồng thời hàmlượng Zn2+ và gluconat trong ba mẫu thực phẩm bảo vệ sức khỏe trên thị trường. Kết quả này cũng đã được đối chứng với phương pháp HPLC-PDA (cho gluconat) và phương pháp ICP-OES (cho Zn2+) cho kết quả khá tương đồng.Nutritional supplements providing bioavailable essential minerals, such as zinc (Zn) and magnesium (Mg), in forms of absorbable salts (e.g., gluconate, stearate, lactate, etc.) have been widely used. However, it should be noted that alongside these supplements, some excipients, including inorganic salts like zinc sulfate and magnesium sulfate, are frequently employed in pharmaceutical and nutraceutical products. Conventional analytical methods for total metal contents could not distinguish actual concentrations of bioavailable forms, suggesting the need for simultaneous analysis of both these essential minerals and their corresponding salts. In this study, we applied the capillary electrophoresis with capacitively coupled contactless conductivity detection (CE-C4D) method to simultaneously measure zinc and gluconate in nutritional supplements. The optimal analytical parameters comprise: (1) 10 mM Tris/Ace electrolyte solution at pH 5.0
(2) silica capillary with an internal diameter of 50 μm and an effective length of 30 cm
(3) separation voltage of +15 kV
(4) hydrodynamic injection mode with siphoning technique at 10 cm height and injection time of 20 s. With these conditions, limit of detections of 1.0 mg/L for zinc and 1.5 mg/L for gluconate were achieved. The method has good repeatability (RSD <
3%) and good recovery (89-103% for zinc and 88-107% for gluconate). The validated method was applied to determine zinc and gluconate concentrations in three commercially available nutritional supplement samples. To ascertain the validity of the results, cross-validation was performed using the high-performance liquid chromatography with photodiode array detection (HPLCPDA) for gluconate and the inductively coupled plasma optical emission spectrometry (ICPOES) for zinc, thereby reinforcing the reliability of the CE-C4D method.

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